CN115533122A - Iron-based alloy body and forming method and application thereof - Google Patents
Iron-based alloy body and forming method and application thereof Download PDFInfo
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- CN115533122A CN115533122A CN202211526921.2A CN202211526921A CN115533122A CN 115533122 A CN115533122 A CN 115533122A CN 202211526921 A CN202211526921 A CN 202211526921A CN 115533122 A CN115533122 A CN 115533122A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 274
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 131
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 91
- 239000000956 alloy Substances 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 107
- 238000002844 melting Methods 0.000 claims abstract description 67
- 230000008018 melting Effects 0.000 claims abstract description 67
- 229910052751 metal Inorganic materials 0.000 claims abstract description 47
- 239000002184 metal Substances 0.000 claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 claims abstract description 41
- 238000007639 printing Methods 0.000 claims abstract description 33
- 238000004088 simulation Methods 0.000 claims abstract description 29
- 210000000988 bone and bone Anatomy 0.000 claims description 88
- 239000007943 implant Substances 0.000 claims description 68
- 239000000758 substrate Substances 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 230000007797 corrosion Effects 0.000 claims description 16
- 238000005260 corrosion Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 229910052748 manganese Inorganic materials 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000003892 spreading Methods 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000009689 gas atomisation Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000004927 fusion Effects 0.000 claims description 2
- 239000011572 manganese Substances 0.000 description 13
- 238000002513 implantation Methods 0.000 description 10
- 210000001124 body fluid Anatomy 0.000 description 7
- 239000010839 body fluid Substances 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- 239000006104 solid solution Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 238000003754 machining Methods 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910000616 Ferromanganese Inorganic materials 0.000 description 1
- 206010061363 Skeletal injury Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/042—Iron or iron alloys
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/58—Materials at least partially resorbable by the body
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/38—Process control to achieve specific product aspects, e.g. surface smoothness, density, porosity or hollow structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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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
- B33Y10/00—Processes of additive manufacturing
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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
- B33Y70/00—Materials specially adapted for additive manufacturing
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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
- B33Y80/00—Products made by additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The application discloses an iron-based alloy body and a forming method and application thereof, relates to the field of metal powder manufactured products, and aims to solve the technical problem that laser selective melting forming parameters matched with a target alloy body structure cannot be obtained in the prior art. The forming method comprises the following steps: preparing iron-based metal powder, and taking the iron-based metal powder as forming powder; based on the formed powder, obtaining selective laser melting forming manufacturing parameters; constructing a simulation model of the target alloy body based on the target alloy body; based on the selective laser melting forming manufacturing parameters, slicing the simulation model of the target alloy body to obtain a printed file; guiding the printing file into selective laser melting forming equipment for printing to obtain a target alloy body; the target alloy body comprises a plurality of unit grids, the rod diameters of the unit grids are 0.12mm-0.20mm, the span of the rod diameters is 2mm-4 mm, and the included angle of the rods is 0-120 degrees.
Description
Technical Field
The application relates to the field of metal powder manufactured products, in particular to an iron-based alloy body and a forming method and application thereof.
Background
The selective laser melting forming is to selectively melt and form metal powder layer by layer, and metal products with complex grids can be manufactured according to a designed three-dimensional model. The metal product of the iron-based complex grid is good in biocompatibility and degradable, but if the metal product is complex, the metal product cannot be manufactured through a conventional machining method, and at present, no technical disclosure about how to select the laser selective melting forming parameters of the iron-based alloy body with a complex structure exists.
Disclosure of Invention
The application mainly aims to provide an iron-based bone implant and a selective laser melting forming method thereof, and aims to solve the technical problem that selective laser melting forming parameters matched with a target alloy body structure cannot be obtained in the prior art.
In order to solve the above technical problem, an embodiment of the present application provides: a method of forming an iron-based alloy body, comprising the steps of:
preparing iron-based metal powder, and taking the iron-based metal powder as forming powder; based on the formed powder, obtaining selective laser melting forming manufacturing parameters;
constructing a simulation model of the target alloy body based on the target alloy body;
based on the selective laser melting forming manufacturing parameters, slicing the simulation model of the target alloy body to obtain a printed file;
guiding the printing file into selective laser melting forming equipment for printing to obtain a target alloy body; the target alloy body comprises a plurality of unit grids, the rod diameters of the unit grids are 0.12mm-0.20mm, the span of the rod diameters is 2mm-4 mm, and the included angle of the rods is 0-120 degrees.
As some optional embodiments herein, the iron-based metal powder comprises: 24 to 28wt% Mn, 8 to 10wt% Si, 2 to 3wt% Cu and 0.6wt% C, the balance Fe;
as some alternative embodiments of the present application, the preparing the iron-based metal powder, the iron-based metal powder as a forming powder; based on the molding powder, obtaining selective laser melting molding manufacturing parameters, which comprise:
preparing first iron-based metal powder by adopting a vacuum gas atomization method;
performing powder sieving treatment and drying treatment on the first iron-based metal powder to obtain second iron-based metal powder;
taking the second iron-based metal powder as a forming powder; and obtaining selective laser melting forming manufacturing parameters based on the forming powder.
As some optional embodiments of the application, the drying temperature of the drying treatment is 150 ℃, the drying time is 6 to 8 hours, and the vacuum pressure is-0.8 to-1.0 bar.
As some optional embodiments of the present application, the laser selective melting forming manufacturing parameters include: the thickness of the powder layer is 20 microns, the diameter of a light spot is 50 microns, the outline is cancelled, only the inner surface is opened, the laser power is 110W-140W, the scanning speed is 950 mm/s-1050 mm/s, the scanning distance is 0.06mm-0.08mm, the strip distance is-0.06 mm, and the path deviation is 0.03mm-0.04mm.
As some optional embodiments of the present application, the importing the print file into a selective laser melting and forming apparatus for printing to obtain a target alloy body includes:
guiding the printed file into selective laser melting forming equipment, mounting a substrate and a scraper, spreading powder, setting the temperature of the substrate, introducing argon for protection, and starting printing to obtain a first target alloy body;
and taking out the first target alloy body, performing powder cleaning treatment, and removing the substrate to obtain the target alloy body.
As some optional embodiments of the present application, the substrate has a roughness value of Ra1.6 μm to Ra3.2 μm, and the substrate heating temperature is 150 ℃.
As some optional embodiments of the present application, the argon purity is 99.999%, the oxygen content in the chamber of the selective laser melting and forming device is less than 200ppm, the pressure in the chamber is 1mbar to 20mbar, and the dedusting air volume is 14 m 3 /h～18 m 3 /h。
In order to solve the above technical problem, the embodiment of the present application further provides: an iron-based alloy body obtained by the forming method described above, said iron-based alloy body being obtained by selective laser melting forming, the formed powder comprising the following components: 24 to 28wt% Mn, 8 to 10wt% Si, 2 to 3wt% Cu and 0.6wt% C, the balance Fe.
In order to solve the above technical problem, the embodiment of the present application further provides: use of an iron-based alloy body for the preparation of an iron-based bone implant; wherein the 30-day body fluid corrosion rate of the iron-based bone implant is 0.25mm/year to 0.32mm/year, and the elastic modulus of the iron-based bone implant is 10 to 18GPa; the unit rod diameter of the iron-based bone implant is 0.12mm-0.2mm, the span of the rod diameter is 2mm-4 mm, and the included angle of the rod is 0-120 degrees.
Compared with the prior art, the iron-based bone implant is manufactured by the selective laser melting forming method, and compared with the traditional processing and manufacturing technology, the selective laser melting forming method does not need a die in the forming process, so that the manufacturing efficiency is greatly improved, and the manufacturing cost is reduced; the alloy body has stronger processability, can produce an alloy body with a complex structure and higher requirement on fineness, namely a target alloy body comprising a plurality of unit grids, wherein the rod diameter of each unit grid is 0.12mm to 0.20mm, the rod diameter span is 2mm to 4mm, and the rod included angle is 0-120 degrees. In practical application, because the composition of the forming powder and the simulation model are different, the forming parameters are often greatly different, and because the specific process parameters are needed to control the laser scanning system to melt the simulation model to form a corresponding cross section based on the properties of the forming powder and the structural characteristics of the simulation model, the laser scanning system is manufactured layer by layer until the product is manufactured completely. Therefore, in a specific application, the iron-based metal powder is prepared and used as a forming powder; based on the formed powder, obtaining selective laser melting forming manufacturing parameters; constructing a simulation model of the target alloy body based on the target alloy body; based on the selective laser melting forming manufacturing parameters, slicing the simulation model of the target alloy body to obtain a printed file; and guiding the printing file into selective laser melting forming equipment for printing to obtain a target alloy body. It can be seen that based on the method of the present application, a forming parameter with a high matching degree can be obtained based on the target alloy body structure.
Drawings
FIG. 1 is a schematic representation of an iron-based bone implant structure according to an embodiment of the present application;
fig. 2 is a block diagram of an iron-based bone implant formed in accordance with example 1 of the present application;
fig. 3 is a block diagram of an iron-based bone implant formed in accordance with example 2 of the present application;
fig. 4 is a structural view of an iron-based bone implant formed in example 3 of the present application.
Detailed Description
It should be understood that the specific embodiments described herein are merely illustrative of and not restrictive on the broad application.
Fracture or bone injury caused by accidents, aging and the like can be treated by implanting a metal splint through operations, but after the bone is healed, metal exists in a human body, and the metal splint needs to be taken out, which causes secondary injury.
The selective laser melting formation is to perform selective laser melting formation layer by layer on the metal powder spread layer by layer, and can manufacture metal products with complex grids according to a designed three-dimensional model, particularly can manufacture products which cannot be manufactured by machining, such as a bone-like structure. The iron-based bone implant has good biocompatibility and is degradable, the imitated bone tissue of the iron-based bone implant is most beneficial to the growth of the bone tissue, but the iron-based bone implant cannot be manufactured by a conventional machining method, the imitated bone tissue can be formed by selective laser melting, and the iron-based bone implant has the elastic modulus (3-20 GPa) which is close to that of the human bone structure and can be formed in a customized manner, so that the manufacturing method of the iron-based bone implant is an ideal iron-based bone implant manufacturing method.
The difficulty of forming the unsupported iron-based profiling bone implantation fine structure (the rod diameter is as small as 0.12 mm) by selective laser melting is that the selective laser melting forming parameters of the temporary unsupported iron-based metal powder material at present can be solved only from the printing manufacturing parameters because the rod diameter of the profiling bone implantation structure is as small as 0.12mm and cannot be supported, and the printing forming parameters of the material need to be optimized first, and then the manufacturing parameters of printing the thin rod diameter are further optimized on the basis, so that the manufacturing method for forming the iron-based bone implantation structure by selective laser melting is found.
The selective laser melting forming is to selectively melt and form metal powder layer by layer, and metal products with complex grids can be manufactured according to a designed three-dimensional model. The metal product with the iron-based complex grid is good in biocompatibility and degradable, but if the metal product is complex, the metal product cannot be manufactured through a conventional machining method, and at present, no technical disclosure about how to select selective laser melting forming parameters of the iron-based alloy body with a complex structure is disclosed.
In order to solve the above technical problem, the embodiment of the present application further provides: a method of forming an iron-based alloy body, comprising the steps of:
s1, preparing iron-based metal powder, wherein the iron-based metal powder is used as forming powder; and obtaining selective laser melting forming manufacturing parameters based on the forming powder.
In a specific application, the preparing of the iron-based metal powder in step S10 includes: preparing first iron-based metal powder by adopting a vacuum gas atomization method; and performing powder sieving treatment and drying treatment on the first iron-based metal powder to obtain a second iron-based metal powder. Wherein the drying temperature of the drying treatment is 150 ℃, the drying time is 6 to 8 hours, and the vacuum pressure is-0.8 to-1.0 bar. The vacuum atomization method is characterized in that high-speed airflow is used for acting on a molten liquid flow, so that the kinetic energy of the gas is converted into the surface energy of the molten liquid, and then fine liquid drops are formed and solidified into powder particles.
In a specific application, the iron-based powder is prepared by a vacuum atomization method, and the iron-based metal powder comprises: 24 to 28wt% Mn, 8 to 10wt% Si, 2 to 3wt% Cu, and 0.6wt% C, the balance being Fe. The Fe is easy to corrode in a physiological environment, has natural degradability, does not generate a hydrogen evolution reaction in a degradation process, and has small influence on the mechanical property of the bone implant; meanwhile, in order to improve the technical problem that the corrosion rate of the iron-based implant is slow in a physiological environment, the iron-based implant is alloyed with Fe by adding Mn, and is dissolved in a Fe matrix in a solid solution mode under the preparation condition of selective laser melting forming to form a solid solution phase with low electrode potential, so that the electrode potential of the whole bone implant is reduced; meanwhile, alloying is carried out on the implant by adding the element Si and the element Cu to form micro-galvanic corrosion; that is, in the embodiments of the present application, by adding Mn, si and Cu simultaneously to the iron matrix, the degradation of the osteoimplant is synergistically accelerated, that is, on one hand, the electrode potential of the osteoimplant is reduced, and a ferro-manganese solid solution is formed, and on the other hand, cu and Si are precipitated along the grain boundary of the austenite phase, and form a plurality of local micro-galvanic corrosion units with the matrix, thereby accelerating the degradation of the osteoimplant in a physiological environment.
And S2, building a simulation model of the target alloy body based on the target alloy body.
And S3, based on the selective laser melting forming manufacturing parameters, slicing the simulation model of the target alloy body to obtain a printed file.
S4, importing the printing file into selective laser melting forming equipment for printing to obtain a target alloy body; the target alloy body comprises a plurality of unit grids, the rod diameter of each unit grid is 0.12mm-0.20mm, the rod diameter span is 2mm-4 mm, and the rod included angle is 0-120 degrees.
In specific application, compared with the prior art, the iron-based bone implant is manufactured by the selective laser melting forming method, and compared with the traditional processing and manufacturing technology, the selective laser melting forming method does not need a die in the forming process, so that the manufacturing efficiency is greatly improved, and the manufacturing cost is reduced; the alloy body has stronger processability, can produce an alloy body with a complex structure and higher requirement on fineness, namely a target alloy body comprising a plurality of unit grids, wherein the rod diameter of each unit grid is 0.12mm to 0.20mm, the rod diameter span is 2mm to 4mm, and the rod included angle is 0-120 degrees. In practical application, because the composition of the forming powder and the simulation model are different, the forming parameters are often greatly different, and because the specific process parameters are needed to control the laser scanning system to melt the simulation model to form a corresponding cross section based on the properties of the forming powder and the structural characteristics of the simulation model, the laser scanning system is manufactured layer by layer until the product is manufactured completely. Therefore, in a specific application, the iron-based metal powder is prepared and used as a forming powder; based on the formed powder, obtaining selective laser melting forming manufacturing parameters; constructing a simulation model of the target alloy body based on the target alloy body; based on the selective laser melting forming manufacturing parameters, slicing the simulation model of the target alloy body to obtain a printed file; and guiding the printed file into selective laser melting forming equipment for printing to obtain a target alloy body. It can be seen that based on the method of the present application, a forming parameter with a high matching degree can be obtained based on the target alloy body structure.
And S20, building a simulation model of the target alloy body based on the target alloy body.
In specific application, a simulation model of the target alloy body is obtained based on the condition of the target alloy body, simulation model design of the parameterized target alloy body is carried out by using ntoology software according to the condition of the target alloy body, the structure of the simulation model of the target alloy body is the same as that of the finally obtained target alloy body, the simulation model of the target alloy body comprises a plurality of unit grids, the rod diameter of each unit grid is 0.12mm-0.20mm, the rod diameter span is 2mm-4 mm, and the rod included angle is 0-120 degrees. The unit grids comprise disordered unit grids and ordered unit grids; the target alloy body structure described in the embodiments of the present application does not require support.
S30, slicing the target alloy body simulation model, and setting selective laser melting forming manufacturing parameters; based on the parameters, a print file is obtained.
In a specific application, the slicing process is completed by magics software without support, and the laser selective area fusion forming manufacturing parameters comprise: the thickness of the powder layer is 20 microns, the diameter of a light spot is 50 microns, the outline is cancelled, only the inner surface is opened, the laser power is 110W-140W, the scanning speed is 950 mm/s-1050 mm/s, the scanning distance is 0.06mm-0.08mm, the strip distance is-0.06 mm, and the path deviation is 0.03mm-0.04mm.
S40, importing the printing file into selective laser melting forming equipment for printing to obtain a target alloy body; the target alloy body comprises a plurality of unit grids; the target alloy body comprises a plurality of unit grids, the rod diameters of the unit grids are 0.12mm-0.20mm, the span of the rod diameters is 2mm-4 mm, and the included angle of the rods is 0-120 degrees.
In a particular application, the target alloy body obtained by the above-described method is used to prepare an iron-based bone implant; wherein the 30-day liquid corrosion rate of the iron-based bone implant is 0.25-0.32mm/year, and the elastic modulus of the iron-based bone implant is 10-18GPa; the unit rod diameter of the iron-based bone implant is 0.12mm-0.2mm, the span of the rod diameter is 2mm-4 mm, and the included angle of the rod is 0-120 degrees.
In a specific application, the step S40 of guiding the print file into a selective laser melting and forming device for printing to obtain a target alloy body includes:
guiding the printed file into selective laser melting forming equipment, mounting a substrate and a scraper, spreading powder, setting the temperature of the substrate, introducing argon for protection, and starting printing to obtain a first target alloy body;
and taking out the first target alloy body, performing powder cleaning treatment, and removing the substrate to obtain the target alloy body.
Wherein the roughness value of the substrate is Ra1.6-Ra3.2 μm, and the heating temperature of the substrate is 150 ℃. As some optional embodiments of the present application, the argon purity is 99.999%, the oxygen content in the chamber of the selective laser melting and forming device is less than 200ppm, the pressure in the chamber is 1mbar to 20mbar, and the dedusting air volume is 14 m 3 /h～18 m 3 H is the ratio of the total weight of the catalyst to the total weight of the catalyst. Wherein, the powder cleaning treatment can be vibration powder cleaning and then flow channel air blowing powder cleaning; the substrate removal may be performed by wire cutting.
According to the selective laser melting forming method, a die is not needed in the forming process, so that the manufacturing efficiency is greatly improved, and the manufacturing cost is reduced; and is more machinable, allowing for the production of bone implants having complex structures and requiring greater precision. Therefore, when the iron-based alloy body is used for preparing a bone implant, a bone implant simulation model is firstly constructed based on the condition of the recipient bone, and the simulation model is sliced by using three-dimensional slicing software to form a plurality of stacked two-dimensional slices; and then putting the prepared iron-based powder into a powder supply cylinder, lifting the iron-based powder in the powder supply cylinder by controlling the height of a piston of the powder supply cylinder, moving and spreading the powder by using a scraper, and uniformly delivering the powder in the powder supply cylinder to a substrate in a forming area and spreading the powder on the substrate. However, in practical applications, because the composition of the forming powder and the simulation model are different, the forming parameters are often greatly different, and because the laser scanning system is controlled to melt the simulation model to form a corresponding cross section by using specific process parameters based on the properties of the forming powder and the structural characteristics of the simulation model, and then the layer-by-layer manufacturing is performed until the product manufacturing is completed.
Based on the above, the embodiment of the application provides an iron-based bone implant, wherein the 30-day body fluid corrosion rate of the iron-based bone implant is 0.25mm/year to 0.32mm/year, and the elastic modulus of the iron-based bone implant is 10 to 18GPa; the unit rod diameter of the iron-based bone implant is 0.12mm-0.20mm, the span of the rod diameter is 2mm-4mm, and the included angle of the rod is 0-120 degrees; in a particular application, the iron-based bone implant may be custom designed according to the condition of the recipient bone.
The iron-based bone implant is obtained by selective laser melting forming, and the forming powder comprises the following components: 24 to 28wt% Mn, 8 to 10wt% Si, 2 to 3wt% Cu and 0.6wt% C, the balance Fe.
When the iron-based alloy body is used for preparing a bone implant, the iron-based bone implant is shown in a schematic structure in fig. 1.
Compared with the prior art, the iron-based bone implant is obtained by selective laser melting and forming, and the forming powder comprises the following components: 24 to 28wt% Mn, 8 to 10wt% Si, 2 to 3wt% Cu and 0.6wt% C, the balance Fe; the Fe is easy to corrode in a physiological environment, has natural degradability, does not generate a hydrogen evolution reaction in a degradation process, and has small influence on the mechanical property of the bone implant; meanwhile, in order to solve the technical problem that the corrosion rate of the iron-based implant is low in a physiological environment, mn and Fe are added for alloying, and the iron-based implant is dissolved in a Fe matrix in a solid solution mode under the preparation condition of selective laser melting forming to form a solid solution phase with low electrode potential, so that the overall electrode potential of the bone implant is reduced; meanwhile, alloying is carried out on the implant by adding the element Si and the element Cu to form micro-galvanic corrosion; that is, the embodiments of the present application add Mn, si and Cu to the iron matrix simultaneously, so that the Mn, si and Cu synergistically accelerate the degradation of the bone implant, that is, on one hand, the electrode potential of the bone implant is reduced to form a fe-Mn solid solution, and on the other hand, cu and Si are precipitated along the grain boundary of the austenite phase to form a plurality of local micro-galvanic corrosion units with the matrix, thereby accelerating the degradation of the bone implant in a physiological environment. The iron-based bone implant provided by the embodiment of the application has a 30-day body fluid corrosion rate of 0.25-0.32 mm/year; the elastic modulus of the iron-based bone implant is 10 to 18GPa; the unit rod diameter of the iron-based bone implant is 0.12mm-0.2mm, the span of the rod diameter is 2mm-4 mm, and the included angle of the rod is 0-120 degrees. Therefore, the degradation performance, the mechanical property and the fineness of the bone implant disclosed by the embodiment of the application can meet the requirements of medical application, and the bone implant can be gradually degraded in vivo while helping the healing of tissues.
The iron-based alloy bodies of the present application, methods of forming the same, and uses thereof, are described in detail below with reference to specific examples, wherein the iron-based alloy bodies of examples 1-3 below are used to make iron-based bone implants.
Example 1
Step 1: preparing iron-based powder by a vacuum gas atomization method, wherein the iron-based powder consists of the following components: 24% of Mn, 10% of Si, 2% of Cu, 0.6% of C and the balance of iron, wherein the total mass percent is 100%; sieving powder before printing, vacuum drying at 150 deg.C for 8 hr under-1.0 bar.
And 2, step: carrying out parametric bone profiling structure model design by using ntology software according to the condition of a receptor bone, designing a profiling bone mesh model file with a unit structure rod diameter of 0.12mm, a rod span of 2-3mm and a rod-rod included angle of 0-120 degrees, importing the file into magics software for optimization, without support, setting laser selective melting forming manufacturing parameters: the thickness of the powder layer is 20 micrometers, the diameter of a light spot is 50 micrometers, the outline is cancelled, only the inner surface is opened, the laser power is 110W, the scanning speed is 950mm/s, the scanning interval is 0.06mm, the strip interval is-0.06 mm, and the path deviation is 0.04mm, and then slicing is carried out to form a slice file.
And step 3: guiding the slice file obtained in the step 2 into selective laser melting forming equipmentLoading a roughened substrate with the roughness of Ra1.6-Ra3.2 mu m, installing a scraper, spreading powder, setting the heating temperature of the substrate at 150 ℃, introducing argon with the purity of 99.999 percent to protect a cavity, wherein the oxygen content in the cavity is less than 200ppm, the pressure in the cavity is 0-20 mbar, and the dedusting air volume is 18 m 3 H, starting printing;
and 4, step 4: after printing, the printing equipment is closed, the cavity door is opened when the temperature in the cavity is reduced to the room temperature, the iron-based bone implantation structural part is taken out and cleaned, the iron-based bone implantation structural part is cleaned by vibration, then the flow channel is blown to clean the powder, and the substrate is removed by linear cutting to obtain the iron-based bone implant 1.
The structure of the iron-based bone implant 1 subjected to selective laser melting forming in the embodiment is shown in fig. 2, and the obtained iron-based bone implant 1 is subjected to elasticity modulus and 30-day human body fluid corrosion rate tests, and the test results are shown in table 1.
Example 2
Step 1: preparing iron-based powder by adopting a vacuum gas atomization method, wherein the iron-based powder comprises the following components: 26% of Mn, 9% of Si, 3% of Cu, 0.6% of C and the balance of Fe, wherein the total mass percent is 100%; sieving powder before printing, vacuum drying at 150 deg.C for 7 hr under-0.9 bar.
And 2, step: carrying out parametric bone profiling structure model design by using ntology software according to the condition of a receptor bone, designing a profiling bone mesh model file with a unit structure rod diameter of 0.2mm, a rod span of 2-4mm and a rod-rod included angle of 0-120 degrees, importing the file into magics software for optimization, without support, setting laser selective melting forming manufacturing parameters: the thickness of the powder layer is 20 micrometers, the diameter of a light spot is 50 micrometers, the outline is cancelled, only the inner surface is opened, the laser power is 120W, the scanning speed is 1000mm/s, the scanning interval is 0.08mm, the strip interval is-0.06 mm, and the path deviation is 0.04mm, and then slicing is carried out to form a slice file.
And step 3: guiding the sliced file obtained in the step 2 into selective laser melting forming equipment, installing a roughened substrate with the roughness of Ra1.6-Ra3.2 mu m, installing a scraper, spreading powder, setting the heating temperature of the substrate to be 150 ℃, introducing argon with the purity of 99.999 percent to protect a cavity, and leading the oxygen content in the cavity to be lower than that in the cavity200ppm, the pressure in the chamber is 0-20 mbar, the dedusting air volume is 16 m 3 H, starting printing;
and 4, step 4: after printing, the printing equipment is closed, the cavity door is opened when the temperature in the cavity is reduced to the room temperature, the iron-based bone implantation structural part is cleaned after being taken out, the iron-based bone implantation structural part is cleaned by vibration, then the flow channel is blown to clean the powder, and the substrate is removed by linear cutting to obtain the iron-based bone implant 2.
The structure of the iron-based bone implant 2 subjected to selective laser melting forming in this embodiment is shown in fig. 3, and the obtained iron-based bone implant 2 is subjected to an elastic modulus and a 30-day human body fluid corrosion rate test, and the test results are shown in table 1.
Example 3
Step 1: preparing iron-based powder by adopting a vacuum gas atomization method, wherein the iron-based powder comprises the following components: 28% of Mn, 8% of Si, 2.5% of Cu, 0.6% of C and the balance of iron, wherein the total mass percent is 100%; sieving before printing, vacuum drying at 150 deg.C for 6 hr under-0.8 bar.
Step 2: carrying out parametric bone profiling structure model design by using ntology software according to the condition of a receptor bone, designing a profiling bone mesh model file with a unit structure rod diameter of 0.20mm, a rod span of 3-4mm and a rod-rod included angle of 0-120 degrees, importing the file into magics software for optimization, without support, setting laser selective melting forming manufacturing parameters: the thickness of the powder layer is 20 microns, the diameter of a light spot is 50 microns, the outline is cancelled, only the inner surface is opened, the laser power is 140W, the scanning speed is 1050mm/s, the scanning interval is 0.08mm, the strip interval is-0.06 mm, and the path deviation is 0.03mm, and then slicing is carried out to form a sliced file.
And 3, step 3: guiding the sliced file in the step 2 into selective laser melting forming equipment, installing a roughened substrate with the roughness of Ra1.6-Ra3.2 mu m, installing a scraper, spreading powder, setting the heating temperature of the substrate to be 150 ℃, introducing argon with the purity of 99.999 percent to protect a cavity, wherein the oxygen content in the cavity is lower than 200ppm, the pressure in the cavity is 0-20 mbar, and the dedusting air volume is 14 m 3 H, starting printing;
and 4, step 4: after printing, the printing equipment is closed, the cavity door is opened when the temperature in the cavity is reduced to the room temperature, the iron-based bone implantation structural member is cleaned after being taken out, the iron-based bone implantation structural member is cleaned by vibration, then the flow channel is blown to clean the powder, and the base plate is removed by linear cutting to obtain the iron-based bone implant 3.
The structure of the iron-based bone implant 3 subjected to selective laser melting forming in this embodiment is shown in fig. 4, and the obtained iron-based bone implant 3 is subjected to an elastic modulus and a 30-day human body fluid corrosion rate test, and the test results are shown in table 1.
Table 1:
it can be seen that the iron-based bone implant obtained by the method of the embodiment of the application is an unsupported iron-based profiling bone implantation fine structure (the rod diameter is as small as 0.12 mm), the structural elastic modulus is 10-18 GPa, the corrosion rate of human body fluid is 0.25-0.32mm/year in 30 days, and the requirements of a degradable metal-based bone implant product on the strength and the corrosion rate of the bone implant can be met.
The above description is only a preferred embodiment of the present application, and not intended to limit the scope of the present application, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the specification and the drawings, or which are directly or indirectly applied to other related technical fields, are included in the scope of the present application.
Claims (10)
1. A method of forming an iron-based alloy body, comprising the steps of:
preparing iron-based metal powder, and taking the iron-based metal powder as forming powder; based on the formed powder, obtaining selective laser melting forming manufacturing parameters;
constructing a simulation model of the target alloy body based on the target alloy body;
based on the selective laser melting forming manufacturing parameters, slicing the simulation model of the target alloy body to obtain a printed file;
guiding the printed file into selective laser melting forming equipment for printing to obtain a target alloy body; the target alloy body comprises a plurality of unit grids, the rod diameter of each unit grid is 0.12mm-0.20mm, the rod diameter span is 2mm-4 mm, and the rod included angle is 0-120 degrees.
2. The method of forming an iron-based alloy body of claim 1, wherein the iron-based metal powder comprises: 24 to 28wt% Mn, 8 to 10wt% Si, 2 to 3wt% Cu and 0.6wt% C, the balance Fe.
3. The iron-based alloy body forming method according to claim 1, wherein the iron-based metal powder is prepared as a forming powder; based on the molding powder, obtaining selective laser melting molding manufacturing parameters, which comprise:
preparing first iron-based metal powder by adopting a vacuum gas atomization method;
performing powder sieving treatment and drying treatment on the first iron-based metal powder to obtain second iron-based metal powder;
taking the second iron-based metal powder as a forming powder; and obtaining selective laser melting forming manufacturing parameters based on the forming powder.
4. A method for forming an iron-based alloy body according to claim 3, wherein the drying temperature is 150 ℃, the drying time is 6 to 8 hours, and the vacuum pressure is-0.8 to-1.0 bar.
5. The method of forming an iron-based alloy body of claim 1, wherein the laser selective fusion forming manufacturing parameters comprise: the thickness of the powder layer is 20 mu m, the diameter of a light spot is 50 mu m, the outline is cancelled, only the inner surface is opened, the laser power is 110W-140W, the scanning speed is 950 mm/s-1050 mm/s, the scanning distance is 0.06mm-0.08mm, the strip distance is-0.06 mm, and the path deviation is 0.03mm-0.04mm.
6. The method for forming an iron-based alloy body according to claim 1, wherein the step of introducing the print file into a selective laser melting forming apparatus for printing to obtain a target alloy body comprises:
guiding the printed file into selective laser melting forming equipment, mounting a substrate and a scraper, spreading powder, setting the temperature of the substrate, introducing argon for protection, and starting printing to obtain a first target alloy body;
and taking out the first target alloy body, performing powder cleaning treatment, and removing the substrate to obtain the target alloy body.
7. The method of forming an iron-based alloy body according to claim 6, wherein the substrate has a roughness value of Ra1.6 μm to Ra3.2 μm, and the substrate heating temperature is 150 ℃.
8. The method for forming the iron-based alloy body according to claim 6, wherein the purity of argon is 99.999%, the oxygen content in a chamber of the selective laser melting and forming device is less than 200ppm, the pressure in the chamber is 1mbar to 20mbar, and the dedusting air volume is 14 m 3 /h～18 m 3 /h。
9. An iron-based alloy body obtained by the forming method according to any one of claims 1 to 8, wherein said iron-based alloy body is obtained by selective laser melting forming and wherein the formed powder comprises the following components: 24 to 28wt% Mn, 8 to 10wt% Si, 2 to 3wt% Cu and 0.6wt% C, the balance Fe.
10. Use of the iron-based alloy body according to claim 9 for the preparation of an iron-based bone implant; wherein the 30-day liquid corrosion rate of the iron-based bone implant is 0.25-0.32mm/year, and the elastic modulus of the iron-based bone implant is 10-18GPa; the unit rod diameter of the iron-based bone implant ranges from 0.12mm to 0.20mm, the span of the rod diameter ranges from 2mm to 4mm, and the included angle of the rod ranges from 0 degree to 120 degrees.
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