CN108165811B - Preparation method of high-strength degradable nano medical porous titanium-magnesium composite material - Google Patents
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Abstract
The invention relates to a preparation method of a degradable nano titanium-magnesium composite material with human affinity and mechanical properties close to those of human bones, in particular to a novel porous titanium-magnesium composite material which is applied to the field of medical implantation. The invention provides a porous titanium-magnesium composite material with a nanocrystalline grain structure, which takes titanium, magnesium, silicon, vanadium and silver as initial components, and the composition of the porous titanium-magnesium composite material can be represented by aTi-bMg-cSi-dV-eAg-f (TiC-SiC-VC), wherein a=40, b=10, c=45, d= 3,e =1.5, f=0.5 and a+b+c+d+e+f=100, and finally the high-strength medical porous titanium-magnesium composite material TiMg-3V-1.5Ag-0.5 (TiC-SiC-VC) porous titanium-magnesium composite material is obtained through a chemical removal method. The nano material with a highly open porous structure is formed, so that the material has mechanical properties similar to those of a human body, magnesium can be slowly and automatically degraded after being implanted into the human body, the possibility of the ingrowth of the original bone tissue of the human body is provided, and the healing of the implanted material and the original bone tissue of the human body is promoted.
Description
Technical Field
The invention relates to a preparation method of a degradable nano titanium-magnesium composite material with human affinity and mechanical properties close to those of human bones, in particular to a novel porous titanium-magnesium composite material which is applied to the field of medical implantation.
Background
The existing metals and alloys used in medicine mainly comprise medical stainless steel, medical cobalt-based alloy, medical titanium and alloys thereof, medical magnesium alloy and other metals and alloys, and the traditional medical metals and alloys have the defects of easy corrosion, possibility of causing diseases due to dissolved ions, causing necrosis of cells and tissues, poor mechanical property, no bioactivity, poor wear resistance, poor fatigue and fracture toughness and the like. And the traditional implants are too stiff, because of this stress shielding, large and rigid femoral prostheses are not recommended for patients with low bone density, which involves bone resorption and bone loss due to a stress shielding. In clinical trials, over 12% of patients suffer moderate or severe bone loss within two years of the implant. The traditional medical material has poor affinity and degradability with human body, bone tissue can not grow inwards, and can not heal with human bone.
Disclosure of Invention
Aiming at the defects of the alloy used in the medical field, the invention aims to reduce the mismatching of an implant body and surrounding bone tissues, realize the rigidity optimization loading of the artificial implant transferred to adjacent bones, and provide a nano material which has good bioactivity, is degradable and has a mechanical property close to that of human bones and has a highly open porous structure.
The invention is realized by the following technical scheme:
the porous titanium-magnesium composite material with the nanocrystalline grain structure provided by the invention takes titanium, magnesium, silicon, vanadium and silver as initial components, the composition of the porous titanium-magnesium composite material can be represented by aTi-bMg-cSi-dV-eAg-f (TiC-SiC-VC), wherein a=40, b=10, c=45, d= 3,e =1.5, f=0.5 and a+b+c+d+e+f=100, and finally the high-strength medical porous titanium-magnesium composite material TiMg-3V-1.5Ag-0.5 (TiC-SiC-VC) porous titanium-magnesium composite material is obtained through a chemical removal method. The porous titanium-magnesium composite material with the nano grain structure has the advantages and is characterized in that: the titanium, magnesium, silicon, vanadium, silver and other components are used as basic components, the human body must contain microelements vanadium and magnesium, wherein the magnesium has good degradability, can be automatically and slowly decomposed after being implanted into the human body, can form a highly open porous structure after being corroded by alkali in the later stage of silicon, and the titanium has reliable hardness conditions, the porous titanium can also have mechanical properties similar to the bones of the human body, the existence of the pores can provide possibility for the ingrowth of bone tissues, and the vanadium can be well combined with the titanium, so that the material has good comprehensive properties. The addition of silver metal makes the material possess broad-spectrum antibiotic property and raise the medical function of the material. The granular material is prepared and then is directly pressed into a blank by bonding with acetone, so that toxic substances are avoided in the traditional metal sintering process, the titanium-magnesium composite material with the nano grain structure can be repeatedly extruded through a three-fork-shaped die channel without taking a piece, the formed nano material is corroded in alkali to form the nano material with the highly open porous structure, the nano material can be slowly and automatically degraded after being implanted into a human body, and the possibility is provided for bone tissue ingrowth and bone tissue healing of the implanted bone and the human body. The invention provides a preparation method of a high-strength porous nano medical degradable titanium-magnesium composite material, which comprises the following steps:
(1) Preparing materials and blanking: cp Ti powder, mg particles (purity 99.6%), si particles (purity 99.9%), V particles (purity 99.9%), ag particles (purity 99.9%) and TiC-SiC-VC whisker particles were taken, the powder blend was weighed in an argon-filled glove box, then mixed with 1% by weight isopropyl alcohol and stirred for 3 minutes. Subsequently, the elemental mixture slurry was taken out of the glove box in a sealed container and poured into a press die inlet passage while blocking an outlet passage by a back pressure punch, the mixture was cold-pressed at 50MPa and dried at room temperature for 5 minutes, isopropyl alcohol was evaporated and adhesion between particles was lost. Finally, a rod-like specimen of D10mm by 68mm was obtained.
(2) Obtaining nano-organization: the method comprises the steps of filling a sample into a sheath, wherein the external dimension of the sheath is D12mm multiplied by 70mm, the internal cavity is D10mm multiplied by 68mm, repeated extrusion can be realized without taking a piece through a three-fork-shaped die channel, and the titanium-magnesium composite material with a nano grain structure is obtained, wherein the extrusion parameters of the three-fork-shaped die channel are as follows: the extrusion speed of the punch is 1mm/s, and the high-strength nano material can be obtained by accumulating enough deformation by rotating the three-fork-shaped die for 6 times.
(3) Forming a material having a highly open porous structure: the rod-shaped nanomaterial produced by the trifurcate mold was immersed in a 5M aqueous sodium hydroxide (NaOH) solution at 60 ℃ for 12 hours to remove Si. Reaction for removal of Si: si (Si) (s) +2NaOH (aq) +H 2 O (aq) ＝Na 2 SiO 3(aq) +2H 2(g)
The porous Ti/Mg composite material from which the Si material was removed was washed in distilled warm water and dried in air for 24 hours, and finally a porous Ti-based composite material having a porosity of 45% was obtained.
The preparation process of the titanium carbide-silicon carbide-vanadium carbide whisker particles in the step (1) comprises the following steps: the titanium oxide-silicon carbide-vanadium carbide whisker precursor material comprises the following chemical components in percentage by weight: v (V) 2 O 5 ：25.4～28.2％，Ti：19.6～19.8％，SiO 2 :25.4 to 28.2 percent, C:20.2 to 22.6 percent, mn:0.1 to 0.9 percent of NaCl:1.0 to 8.1 percent. Adding absolute ethyl alcohol into precursor composite powder which is prepared according to a proportion and can generate titanium carbide-silicon carbide-vanadium carbide whiskers, mechanically ball-milling for 48 hours in a ball mill to obtain superfine precursor composite powder with 200-600nm grain size, filling the powder into a graphite container, and preserving the temperature for 90-180 min under the protection of argon atmosphere and at the temperature of 1550-1800 ℃ to synthesize the titanium carbide-silicon carbide-vanadium carbide whisker.
SiO 2 +2c= (heating) si+2co+.
Si+c= (heating) SiC
V 2 O 5 +7c= (heating) 2vc+5co+.
Ti+c= (heating) TiC
The invention adopts titanium carbide-silicon carbide-vanadium carbide reinforced degradable nano medical porous titanium magnesium composite material, which is characterized in that: the material is formed by directional arrangement of titanium carbide-silicon carbide-vanadium carbide whiskers and titanium magnesium composite material matrix material along extrusion streamline, and the whisker diameter is 200-800nm.
The invention provides a preparation method of a high-strength nano medical degradable titanium-magnesium composite material, which has the advantages that compared with the existing medical alloy:
1. firstly, the formulation is innovated: titanium, magnesium, silicon and vanadium are mixed according to a certain proportion, wherein CPTi is selected instead of the conventional titanium-magnesium composite material, because TiC alloy elements are not released in vivo, titanium is an element which can ionize cells through the radiation of consistent wavelength to regulate human body current, so that the physiological effect beneficial to human bodies is generated, the titanium has excellent mechanical property, corrosion resistance and biocompatibility, can provide enough mechanical strength, and has the mechanical property similar to human bones by forming a highly open porous structure; mg and V are microelements necessary for human body, and vanadium can be well combined with titanium; mg powder and Si powder are taken as space materials, neither magnesium nor silicon can cause cytotoxicity, and the magnesium has the advantages of mildness, absorbability, good biocompatibility and the like, the silicon can be corroded by alkali in the later period to form a material with a highly open porous structure, the degradation behavior of the magnesium enables the magnesium to become a biodegradable implant material, the magnesium can be automatically degraded in a human body after implantation, and the possibility is provided for bone tissue ingrowth and bone and human bone tissue healing after implantation.
2. The following innovation of the manufacturing process flow:
(a) The granular materials are uniformly prepared, bonded by isopropanol and then directly pressed to form a blank, so that the defect that toxic substances can be generated in the traditional metal smelting and sintering process is overcome.
(b) And a three-fork-shaped mold channel is adopted, repeated extrusion can be completed without taking a piece, and the sample is subjected to severe plastic deformation, so that the titanium-magnesium composite material with a nano grain structure is obtained. The obtained nano material has the advantages of high strength, good toughness, good mechanical property, good fatigue resistance and corrosion resistance, degradability and the like.
3. Innovations of forming material morphology structures: the nano material formed by processing is added with alkali to corrode silicon, and magnesium can be automatically degraded in human body in later period to form the nano material with a highly open porous structure, so that the material has mechanical property similar to that of human body, and magnesium can be slowly and automatically degraded after being implanted into human body, thereby providing possibility for the ingrowth of original bone tissue of the body and promoting the healing of the implanted material and the original bone tissue of the body.
4. The preparation method provided by the invention has the advantages of simple process, easiness in realizing large-scale automatic production and capability of being used in the field of medical implantation.
Description of the drawings:
the following is a detailed description of specific embodiments of the invention with reference to the drawings and examples.
FIG. 1 is a schematic illustration of a press molding process after uniformly mixing and bonding particulate materials;
FIG. 2 is a schematic view of a molded rod-shaped test specimen;
FIG. 3 is a schematic illustration of the preparation of a titanium magnesium composite material with nanocrystalline grain structure by repeated extrusion deformation through a three-fork mold tunnel in an embodiment of the invention;
FIG. 4 is a schematic illustration of a rod-shaped material treated with alkali to form a porous material;
the labels in the above figures are:
FIG. 1 is a schematic illustration of a particulate material being uniformly mixed and formed by compression with high pressure.1. Press top cover 2. Press cavity 3. Press bottom cover 4. Rod-shaped sample extrusion channel.
FIG. 2 is a schematic view of a molded stick-shaped specimen, 1. A cover slip 2. A cover 3. A specimen.
FIG. 3 is a schematic diagram of a device for preparing a titanium-magnesium composite material with a nano-grain structure by repeated extrusion deformation through a three-fork-shaped mold channel in an embodiment of the invention, wherein the schematic diagram comprises a male mold, a extrusion blank, a rotary female mold, a prestress clamp, a push rod, a back pressure push rod and a prestress clamp base.
Fig. 4 is a schematic illustration of a rod-shaped material treated with alkali to form a porous material, beaker 2.Naoh solution 3. Rod-shaped nanomaterial.
The specific embodiment is as follows:
example one: the preparation method of the high-strength nano medical porous titanium magnesium composite material comprises the steps of uniformly mixing Ti powder, mg particles (the purity is 99.6%), si particles (the purity is 99.9%), V particles, ag particles and TiC-SiC-VC whisker particles according to the molar ratio of 40:10:45:3:1.5:0.5, bonding by isopropanol, extruding by a press machine die, drying at room temperature for 5 minutes, evaporating the isopropanol, and eliminating the adhesion between the particles to finally form a rod-shaped sample with the D10mm multiplied by 68 mm; the rod-shaped sample is put into a sheath and repeatedly rotated through a three-fork-shaped channel, extruded for 6 times, and subjected to severe plastic deformation to obtain the titanium-magnesium composite material with the nano grain structure, the rod-shaped nano material produced through the three-fork-shaped mould channel is put into a 5L sodium hydroxide (NaOH) aqueous solution at 60 ℃ for soaking for 12 hours to remove Si, washed and ultrasonically cleaned by distilled warm water, then washed by distilled warm water and dried in air for 24 hours, and finally the porous titanium-based composite material with 45% porosity is obtained. The Ti-10Mg-45Si-3V-1.5Ag-0.5 (TiC-SiC-VC) titanium magnesium composite material with the nano grain structure provided by the invention can be prepared by adopting simple metal pressure processing equipment, and then the high-strength nano Ti-3V-1.5Ag-0.5 (TiC-SiC-VC) titanium magnesium porous composite material is obtained by a chemical removal method, so that the obtained porous nano material has mechanical properties similar to those of human bones, and has reliable mechanical hardness and strength and good toughness. And the material has good degradability, so that the material has potential application value and can be used in the field of medical implantation.
Claims (1)
1. A preparation method of a high-strength medical nano porous titanium magnesium composite material is characterized by comprising the following steps: mixing granular materials according to a certain proportion, bonding the granular materials by isopropanol, directly carrying out powder pressing to form a blank, repeatedly extruding the blank through a three-fork-shaped die channel without taking a piece to generate severe plastic deformation, accumulating enough equivalent strain to refine grains, obtaining a high-strength material with a nano grain structure, and then placing the nano material into sodium hydroxide aqueous solution to corrode the silicon to form the nano material with a highly open porous structure;
(a) The porous titanium-magnesium composite material with the nano grain structure takes titanium, magnesium, silicon, vanadium and silver as initial components, the composition of the porous titanium-magnesium composite material is represented by aTi-bMg-cSi-dV-eAg-f (TiC-SiC-VC), wherein a=40, b=10, c=45, d=3, e=1.5, f=0.5 and a+b+c+d+e+f=100, and finally the high-strength medical nano porous titanium-magnesium composite material TiMg-3V-1.5Ag-0.5 (TiC-SiC-VC) is obtained through a chemical removal method;
(b) Uniformly preparing the metal particle initial components provided in the step (a) according to a proportion, weighing the powder blend in an argon-filled glove box, mixing with 1% isopropanol by weight and stirring for 3 minutes; subsequently, the mixture slurry was taken out of the glove box in the sealed container and poured into the inlet passage of the press mold while blocking the outlet passage by the back pressure punch, the mixture was cold-pressed at 50MPa and dried at room temperature for 5 minutes, isopropyl alcohol was evaporated and the adhesion between particles disappeared; finally processing into a rod-shaped sample with the diameter of D10mm multiplied by 68 mm;
(c) The metal particle component provided by the step (a) is subjected to compression forming, and repeated severe plastic deformation is completed without taking a piece through a three-fork-shaped die channel, so that the high-strength titanium-magnesium composite material with a nano grain structure is obtained; the repeated extrusion processing parameters of the channel are as follows: the extrusion speed of the punch is 1mm/s, and the high-strength nano material is obtained by rotating the three-fork-shaped die for 6 times to accumulate enough deformation;
(d) The rod-shaped test piece formed by the metal particle component provided in the step (a) is soaked in 5L of sodium hydroxide aqueous solution at 60 ℃ for 12 hours to remove Si, then distilled warm water is used for washing and is dried in air for 24 hours, and finally the porous titanium magnesium composite material with 45% porosity is obtained.
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| CN111266592B (en) * | 2020-03-25 | 2022-04-22 | 燕山大学 | Titanium-magnesium composite material with double-communication structure and preparation method and application thereof |
| CN111996404B (en) * | 2020-08-21 | 2021-11-12 | 中南大学 | Titanium-based alloy with both quantitative magnesium loading and slow magnesium ion release functions and preparation method and application thereof |
| CN115969551A (en) * | 2023-02-20 | 2023-04-18 | 北京华益圣亚医疗器械有限公司 | Oral implant and manufacturing method thereof |
| CN118080855B (en) * | 2024-04-28 | 2024-06-21 | 合肥工业大学 | In-situ forming device for Y-shaped piece of aluminum-based composite material |
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| CN101948964A (en) * | 2010-09-16 | 2011-01-19 | 大连理工大学 | Method for preparing biomedical porous titanium and titanium alloy material |
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| CN101098916A (en) * | 2005-01-13 | 2008-01-02 | 金文申有限公司 | Composite materials containing carbon nanoparticles |
| CN102481558A (en) * | 2009-05-28 | 2012-05-30 | 国立科学研究中心 | Use Of A Porous Crystalline Hybrid Solid As A Nitrogen Oxide Reduction Catalyst And Devices |
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