CN115501386A - Full-degradable high-toughness bionic gradient composite material and additive manufacturing method thereof - Google Patents
Full-degradable high-toughness bionic gradient composite material and additive manufacturing method thereof Download PDFInfo
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Abstract
The invention provides a fully-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof, and relates to the field of medical material preparation. The fully-degradable high-toughness bionic gradient composite material and the additive manufacturing method thereof specifically comprise the following steps: s1, selecting raw materials, selecting and preparing two different degradable metal materials as a framework and a casting layer respectively, wherein the selected metal materials can be two different materials of zinc-based metal, magnesium-based metal, iron-based metal or molybdenum-based metal, S2, drying the metal raw materials, S3, preparing a framework substrate, S4, manufacturing a three-dimensional model, S5, manufacturing the framework in an additive mode, S6, separating and polishing the framework, S7, preparing a casting mould, S8, casting an outer layer, and S9, demoulding, grinding and polishing finished products. The invention provides a fully-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof.
Description
Technical Field
The invention relates to the field of medical material preparation, in particular to a fully-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof.
Background
The bone repair material is generally a device and a material implanted into a human body through an operation to repair bone defects, belongs to biomedical materials, and puts higher requirements on the bone repair material along with the increase of bone defect cases, the bone repair material also becomes one of the more popular research subjects in the field of biomedical materials, and in the composite biomaterial, an inorganic composite material is the most extensive one in application research and is mainly used as a bone repair or bone fixation material.
The existing degradable metal materials for bone repair generally need to have high strength and toughness, however, the strength and toughness of the materials usually show the characteristics of trade-off, meanwhile, the existing part of metal materials are inert metal materials, the composition components of the metal materials are greatly different from apatite microcrystal in human bones in terms of size, composition and structure, and the metal materials cannot be degraded by human bodies, so that the situation that the metal materials are finally absorbed and utilized by the human bodies is not good, and the immune reaction or related immune syndromes of the human bodies can be caused for a long time, therefore, how to provide a fully-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof are particularly important in the current production and living environment.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a fully-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof, and solves the problems that the strength and toughness of the existing material are usually shown to be equivalent to those of the existing material, the existing material is difficult to have the characteristics of high strength and high toughness, the degradation rate is inconvenient to control, and the bioactivity is poor.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a full-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof specifically comprise the following steps:
s1, selecting raw materials
Selecting and preparing two different degradable metal materials as a framework and a casting layer respectively, wherein the selected metal materials can be two different materials of zinc-based metal, magnesium-based metal, iron-based metal or molybdenum-based metal;
s2, drying the metal raw material
Processing one of the two selected metal raw materials as a raw material for manufacturing a framework into metal powder, and heating and drying the two raw materials in a vacuum drying oven;
s3, preparing a skeleton substrate
Selecting an alloy with the same components as the metal powder material for manufacturing the framework as a substrate, and carrying out preheating treatment on the substrate;
s4, manufacturing a three-dimensional model
Determining the finished shape of the composite material according to the three-dimensional model and the clinical diagnosis result, designing the three-dimensional model of a finished product by using three-dimensional drawing software, designing the basic shape of the framework and the porous structure of the framework by using the three-dimensional drawing software, and storing the three-dimensional model in an STL format;
s5. Framework additive manufacturing
Importing the three-dimensional model in the STL format into layered software, adding supports and carrying out slicing processing, setting printing parameters, generating a printing file, transmitting the printing file to a metal printer, setting fusion printing parameters of the metal printer and printing;
s6, separating and polishing the framework
Separating the printed skeleton from the substrate to obtain a skeleton finished product, and polishing the skeleton by adopting an alcohol solution of hydrochloric acid, nitric acid or other acids;
s7, preparing a casting mold
Preparing a corresponding casting mold according to the properties of the selected metal material by utilizing a three-dimensional model of a finished product made by three-dimensional drawing software according to the finished shape of the composite material;
s8, outer layer casting
Preheating the selected metal material to be heated and melted, placing a framework in a mould, casting, and controlling the temperature of the mould during casting;
s9, demoulding, grinding and polishing finished products
And (3) after the finished product is completely cooled to room temperature, demolding the finished product, removing burrs of the finished product by using a milling machine, polishing the surface of the finished product to be smooth, and polishing the finished product by using an alcohol solution of hydrochloric acid, nitric acid or other acids to finish the preparation of the finished product.
Preferably, the heating temperature in the S2 is 60-150 ℃, and the drying time is 3-6 hours.
Preferably, the preheating treatment temperature in the S3 is 50-800 ℃.
Preferably, the fusing printing parameters of the metal printer in S5 are: the diameter of a laser spot is 50-100 mu m, the laser power is 50-200W, the laser scanning speed is 100-2000mm/s, the laser filling interval is 50-80% of the width of a molten pool, the powder spreading thickness is 20-70 mu m, and the included angle of the adjacent powder spreading layers in the laser scanning direction is 45-90 degrees.
Preferably, the volume concentration of the hydrochloric acid, the nitric acid or other acids in the alcohol in the S6 and the S9 ranges from 1% to 5%, and the volume ratio of the hydrochloric acid, the nitric acid or other acids is 1.
Preferably, in S8, the magnesium-based metal melting temperature is 650 ℃, the zinc-based metal melting temperature is 419.5 ℃, the iron-based metal melting temperature is 1538 ℃, the molybdenum-based metal melting temperature is 2620 ℃, and the protective gas is introduced when the magnesium-based metal temperature reaches 350 ℃, the zinc-based metal temperature reaches 350 ℃, the iron-based metal temperature reaches 450 ℃, and the molybdenum-based metal temperature reaches 500 ℃, wherein the protective gas is sulfur hexafluoride and nitrogen.
Preferably, in S8, the mold temperature should be controlled to be 250 ℃ to 300 ℃ regardless of the selected metal material.
Preferably, in S9, the finished product needs to be cooled to room temperature for 24 hours to 72 hours according to the selected metal.
(III) advantageous effects
The invention provides a fully-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof.
The method has the following beneficial effects:
1. compared with the existing high-toughness bionic gradient composite material and the preparation method thereof, the material and the method prepare the porous degradable metal bracket through additive manufacturing, the other degradable metal material is melted and then cast in the porous bracket to form the composite material, and the strength and the toughness of the degradable metal material are improved through the gradient bionic composite material, so that the stability of the composite material in the use process is ensured.
2. The invention provides a fully-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof, the bionic gradient composite material prepared by the material and the method has higher strength and toughness compared with the traditional material, is suitable for more different use environments, has good adaptability to human tissues and body fluids, is nontoxic, does not cause allergy and abnormal metabolism, has no irritation to the tissues, and simultaneously has the advantages that a part of ions can be metabolized and fused into the in-vivo biological environment, and can not influence the biological enzymes.
3. The invention provides a fully-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof.
Drawings
FIG. 1 is a schematic view of a bone plate made in accordance with the present invention;
FIG. 2 is a schematic view of a bone plate made in accordance with the present invention;
fig. 3 is a schematic view of the casting layer of a bone plate made in accordance with the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example (b):
as shown in fig. 1-3, an embodiment of the present invention provides a fully-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof, specifically including the following steps:
s1, selecting raw materials
Two different degradable metal materials are selected and prepared to be respectively used as a framework and a casting layer, the selected metal materials can be two different types of zinc-based metal, magnesium-based metal, iron-based metal or molybdenum-based metal, the two different metals need different processing modes, one metal material is made into an internal framework through additive manufacturing, the other metal material is attached to the framework as the casting layer in a fusion casting mode, the combination of the two materials can improve the strength and the toughness, and the degradation rate can be regulated and controlled, so that the material can be controlled in the using process, the using effect is improved, meanwhile, the material has good adaptability to human tissues and body fluids, is nontoxic, does not cause allergic reaction and abnormal metabolism, and has no irritation to the tissues, and meanwhile, part of ions can be metabolized and can be fused into the in vivo biological environment, the influence on biological enzymes can not be generated, the degradation rate can be regulated and controlled, the metal of the casting material is preferentially degraded, the internal framework is degraded later, the material can be controlled in the using process, and the using effect is improved;
s2, drying metal powder
One of the two selected metal raw materials is used as a raw material for manufacturing the framework and is processed into metal powder, so that the metal powder is convenient to further process and print, the two raw materials are heated and dried in a vacuum drying oven, pores are prevented from being formed inside the material during additive manufacturing and casting, and the quality of a finished product is improved;
s3, preparing a skeleton substrate
The alloy with the same components as the metal powder material for manufacturing the framework is selected as the substrate, the substrate is subjected to preheating treatment, the temperature of the treatment needs to be paid attention to during the preheating treatment, the direct reaction of metal and air is avoided, the use of raw materials is prevented from being influenced, the substrate is favorable for providing a support base for the framework preparation, and the subsequent separation of the substrate and the framework is facilitated;
s4, manufacturing a three-dimensional model
Determining the finished shape of the composite material according to the three-dimensional model and a clinical diagnosis result, designing the three-dimensional model of a finished product by using three-dimensional drawing software, designing the basic shape of a framework and the porous structure of the framework by using the three-dimensional drawing software, facilitating the determination of the shape of the finished product, storing the three-dimensional model in an STL format, enabling the model to be mutually used among a plurality of pieces of software, and being beneficial to providing a foundation for additive manufacturing;
s5. Framework additive manufacturing
The three-dimensional model in the STL format is led into layering software, supports are added and slicing is carried out, deformation of the printed framework due to material accumulation is avoided, printing parameters are set, a printing file is generated and transmitted to a metal printer, and the melting printing parameters of the metal printer are set and printed, so that the framework is integrally formed, and the integrity and the stability of the framework structure are improved;
s6, separating and polishing the framework
Separating the printed skeleton from the substrate to obtain a skeleton finished product, and polishing the skeleton by adopting an alcohol solution of hydrochloric acid, nitric acid or other acids, so that the surface smoothness of the skeleton is favorably improved, and the subsequent further processing is facilitated;
s7, preparing a casting mold
According to the finished shape of the composite material, the shape of the finished product and a user are confirmed by utilizing a three-dimensional model of the finished product manufactured by three-dimensional drawing software, and after the situation that no fault exists is ensured, a corresponding casting mold is prepared according to the properties of the selected metal material, so that the completeness and the stability of the finished product are improved;
s8, outer layer casting
The selected metal material is preheated to be heated and melted, the framework is placed in the mold for casting, so that the framework and the casting layer are fused better, the temperature of the mold is controlled during casting, the one-step casting molding of a finished product is facilitated, and the phenomenon that a joint is left during splicing to cause unstable structure is avoided;
s9, demolding, grinding and polishing finished products
And after the finished product is completely cooled to room temperature, demolding the finished product, removing burrs of the finished product by using a milling machine, polishing the surface of the finished product, improving the quality of the finished product, polishing the finished product by using an alcohol solution of hydrochloric acid, nitric acid or other acids to finish the preparation of the finished product, facilitating the improvement of the surface smoothness of the finished product, enhancing the adaptability of the finished product to a human body and improving the use experience of a user.
The heating temperature in S2 is 60-150 ℃, the drying time is 3-6 hours, the raw materials are favorably ensured to be completely heated and dried, the preheating treatment temperature in S3 is 50-800 ℃, the printing effect of subsequent additive manufacturing is favorably improved, the adhesion of the materials to the substrate is facilitated, and the melting printing parameters of the metal printer in S5 are as follows: the diameter of a laser spot is 50-100 mu m, the laser power is 50-200W, the laser scanning speed is 100-2000mm/S, the laser filling interval is 50-80% of the width of a molten pool, the powder laying thickness is 20-70 mu m, the included angle of the laser scanning directions between adjacent powder laying layers is 45-90 degrees, the metal printer can be ensured to finish the additive manufacturing of a framework, the volume concentration range of hydrochloric acid, nitric acid or other acids in alcohol in S6 and S9 is 1-5 percent, the volume ratio of the hydrochloric acid, the nitric acid or other acids is 1, the smoothness of a finished product and the surface of the framework can be improved, the using effect can be improved, in S8, the magnesium-based metal melting temperature is 650 ℃, the zinc-based metal melting temperature is 419.5 ℃, the iron-based metal melting temperature is 1538 ℃, the melting temperature of the molybdenum-based metal is 2620 ℃, protective gas is needed to be introduced when the temperature of the magnesium-based metal reaches 350 ℃, the temperature of the zinc-based metal reaches 350 ℃, the temperature of the iron-based metal reaches 450 ℃, and the temperature of the molybdenum-based metal reaches 500 ℃, the protective gas is sulfur hexafluoride and nitrogen, which is beneficial to avoiding high-temperature oxidation of each metal and property change, no matter which metal material is selected in S8, the temperature of the die is controlled to be 250-300 ℃, which is beneficial to improving the casting effect of each metal material, avoiding adhesion of a finished product and the die and facilitating subsequent die removal, and the finished product is cooled to room temperature for 24-72 hours according to different selected metals in S9, which is beneficial to avoiding the danger of die removal when the temperature is too high.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A full-degradable high-toughness bionic gradient composite material and an additive manufacturing method thereof are characterized by comprising the following steps:
s1, selecting raw materials
Selecting and preparing two different degradable metal materials as a framework and a casting layer respectively, wherein the selected metal materials can be two different materials of zinc-based metal, magnesium-based metal, iron-based metal or molybdenum-based metal;
s2, drying the metal raw material
Processing one of the two selected metal raw materials as a raw material for manufacturing a framework into metal powder, and heating and drying the two raw materials in a vacuum drying oven;
s3, preparing a skeleton substrate
Selecting an alloy with the same component as the metal powder material for manufacturing the framework as a substrate, and carrying out preheating treatment on the substrate;
s4, manufacturing a three-dimensional model
Determining the finished shape of the composite material according to the three-dimensional model and the clinical diagnosis result, designing the three-dimensional model of a finished product by using three-dimensional drawing software, designing the basic shape of the framework and the porous structure of the framework by using the three-dimensional drawing software, and storing the three-dimensional model in an STL format;
s5. Framework additive manufacturing
Importing the three-dimensional model in the STL format into layered software, adding supports and carrying out slicing processing, setting printing parameters, generating a printing file, transmitting the printing file to a metal printer, setting fusion printing parameters of the metal printer and printing;
s6, separating and polishing the framework
Separating the printed skeleton from the substrate to obtain a skeleton finished product, and polishing the skeleton by adopting an alcohol solution of hydrochloric acid, nitric acid or other acids;
s7, preparing a casting mold
Preparing a corresponding casting mold according to the properties of the selected metal material by utilizing a three-dimensional model of a finished product made by three-dimensional drawing software according to the finished shape of the composite material;
s8, outer layer casting
Preheating the selected metal material to be heated and melted, placing the framework in a mould, casting, and controlling the temperature of the mould during casting;
s9, demolding, grinding and polishing finished products
And (3) after the finished product is completely cooled to room temperature, demolding the finished product, removing burrs of the finished product by using a milling machine, polishing the surface of the finished product, and polishing the finished product by using an alcohol solution of hydrochloric acid, nitric acid or other acids to finish the preparation of the finished product.
2. The fully-degradable high-strength and toughness bionic gradient composite material and the additive manufacturing method thereof according to claim 1 are characterized in that: the heating temperature in the S2 is 60-150 ℃, and the drying time is 3-6 hours.
3. The fully-degradable high-strength and toughness bionic gradient composite material and the additive manufacturing method thereof according to claim 1 are characterized in that: the preheating treatment temperature in the S3 is 50-800 ℃.
4. The fully degradable high-toughness bionic gradient composite material and the additive manufacturing method thereof as claimed in claim 1, is characterized in that: and in S5, the melting printing parameters of the metal printer are as follows: the diameter of a laser spot is 50-100 mu m, the laser power is 50-200W, the laser scanning speed is 100-2000mm/s, the laser filling interval is 50-80% of the width of a molten pool, the powder spreading thickness is 20-70 mu m, and the included angle of the adjacent powder spreading layers in the laser scanning direction is 45-90 degrees.
5. The fully-degradable high-strength and toughness bionic gradient composite material and the additive manufacturing method thereof according to claim 1 are characterized in that: the volume concentration range of hydrochloric acid, nitric acid or other acids in the S6 and S9 in the alcohol is 1-5%, and the volume ratio of the hydrochloric acid, the nitric acid or other acids is 1.
6. The fully-degradable high-strength and toughness bionic gradient composite material and the additive manufacturing method thereof according to claim 1 are characterized in that: in S8, the magnesium-based metal melting temperature is 650 ℃, the zinc-based metal melting temperature is 419.5 ℃, the iron-based metal melting temperature is 1538 ℃, the molybdenum-based metal melting temperature is 2620 ℃, and when the magnesium-based metal temperature reaches 350 ℃, the zinc-based metal temperature reaches 350 ℃, the iron-based metal temperature reaches 450 ℃, and the molybdenum-based metal temperature reaches 500 ℃, protective gas needs to be introduced, wherein the protective gas is sulfur hexafluoride and nitrogen.
7. The fully-degradable high-strength and toughness bionic gradient composite material and the additive manufacturing method thereof according to claim 1 are characterized in that: in S8, the temperature of the die is controlled to be 250-300 ℃ no matter what metal material is selected.
8. The fully-degradable high-strength and toughness bionic gradient composite material and the additive manufacturing method thereof according to claim 1 are characterized in that: and in the step S9, the finished product needs to be cooled to room temperature for 24 to 72 hours according to different selected metals.
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