CN110343894B - Porous titanium based on vacuum in-situ hot melting reaction, preparation method and application thereof - Google Patents

Porous titanium based on vacuum in-situ hot melting reaction, preparation method and application thereof Download PDF

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CN110343894B
CN110343894B CN201910734381.9A CN201910734381A CN110343894B CN 110343894 B CN110343894 B CN 110343894B CN 201910734381 A CN201910734381 A CN 201910734381A CN 110343894 B CN110343894 B CN 110343894B
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titanium
porous
vacuum
porous titanium
substrate
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CN110343894A (en
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刘冠鹏
李玉龙
雷敏
王文琴
李学文
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Nanchang University
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Nanchang University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/04Metals or alloys
    • A61L27/06Titanium or titanium alloys
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54Biologically active materials, e.g. therapeutic substances
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/56Porous materials, e.g. foams or sponges
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/08Alloys with open or closed pores
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A61L2300/104Silver, e.g. silver sulfadiazine
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404Biocides, antimicrobial agents, antiseptic agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/02Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/12Materials or treatment for tissue regeneration for dental implants or prostheses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/24Materials or treatment for tissue regeneration for joint reconstruction

Abstract

The invention discloses porous titanium based on vacuum in-situ hot melting reaction, a preparation method and application thereof, wherein the preparation method comprises the following steps: selecting a TA2 pure titanium metal plate with a smooth surface, and cutting, grinding and polishing to prepare a sheet-shaped substrate; placing a pure silver sheet in the center of a prepared TA2 substrate; placing the mixture in a high-temperature vacuum heating furnace, and heating the mixture in vacuum; according to the invention, silver is subjected to in-situ reaction on the surface of pure titanium by adopting a hot melting reaction method, and a porous structure with a micro-nano scale is finally formed; the porous titanium not only has the excellent characteristics of titanium, but also has the characteristics of small density, large specific area, good energy absorption and the like of the metal porous material; the method has the advantages of flexible process, simple operation, low cost and excellent performance of the prepared titanium with the porous structure, and can be widely applied to the fields of biomedical engineering and the like.

Description

Porous titanium based on vacuum in-situ hot melting reaction, preparation method and application thereof
Technical Field
The invention relates to the technical field of biomedical engineering materials, in particular to porous titanium based on vacuum in-situ hot melting reaction, a preparation method and application thereof.
Background
TA2 is industrial pure titanium, has single alpha phase structure and better comprehensive mechanical property. TA2 has been widely used in biomedical engineering, especially in bone repair field, because of its excellent corrosion resistance, biocompatibility, high plasticity and high specific strength. However, the elastic modulus of titanium is not matched with that of natural bone, so that the bone around the implant is seriously weakened, bone resorption around the implant occurs, and finally the implant is loosened and broken to fail. The introduction of pores of the porous titanium obviously reduces the elastic modulus of the titanium, so that the elastic modulus of the porous titanium is matched with that of bone under certain conditions, and the porous titanium also has mechanical properties similar to that of the bone and a unique porous structure; these advantageous features have made porous titanium rapidly an important orthopedic implant material and bone defect repair material.
Therefore, research on the preparation of porous titanium is very important. At present, commonly used techniques for preparing porous structure titanium include powder sintering, deposition, slurry foaming, 3D printing, and the like. The powder sintering method cannot control the size of the porous structure and easily generates stress concentration at the tip of the void, resulting in cracks. The connection strength between the pores prepared by the deposition method and the slurry foaming method is low, and cracks are easily generated in the product. The 3D printing technology has the problems that printing equipment is expensive, requirements on the sphericity and the size of powder are high, cracks and thermal stress often occur in printing, and the like. Although these techniques play an important role in their respective fields, they all have more or less certain limitations.
Disclosure of Invention
The invention aims to provide porous titanium based on vacuum in-situ hot melting reaction, a preparation method and application thereof, aiming at the defects of the prior art.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of porous titanium based on vacuum in-situ hot melting reaction, which comprises the following steps:
(1) pretreating a pure titanium metal plate to obtain a TA2 substrate;
(2) and (3) placing the pure silver sheet in the center of the prepared TA2 substrate, and heating the pure silver sheet in a vacuum environment to realize the in-situ reaction between silver and titanium, thereby obtaining the porous titanium.
As a further improvement of the invention, the pretreatment of the pure titanium metal plate comprises cutting, grinding and polishing.
As a further improvement of the present invention, the TA2 substrate is a sheet substrate.
As a further improvement of the invention, the TA2 substrate has the size of 10mm multiplied by 0.5 mm; the pure silver sheet is circular, the diameter of the pure silver sheet is 5mm, and the thickness of the pure silver sheet is 100 mu m.
As a self-service hairIn a clear further improvement, the vacuum degree of the vacuum environment is 1E-4~5E-5Pa。
As a further improvement of the invention, the heating temperature is 1000-1050 ℃, and the heat preservation time is 1-4 min.
The invention also provides porous titanium prepared by the preparation method of the porous titanium based on the vacuum in-situ hot melting reaction.
The invention also provides application of the porous titanium in biomedicine.
As a further improvement of the invention, the application is the application of porous titanium in artificial teeth, bones and joint systems.
The invention discloses the following technical effects:
according to the invention, silver is subjected to in-situ reaction on the surface of pure titanium by adopting a hot melting reaction method, and a porous structure with a micro-nano scale is finally formed; the porous titanium not only has the excellent characteristics of titanium, but also has the characteristics of small density, large specific area, good energy absorption and the like of the metal porous material; the preparation method has the advantages of flexible process, simple operation, low cost and excellent performance of the prepared titanium with the porous structure, and can be widely applied to the fields of biomedical engineering and the like.
According to the invention, Ag is wetted and spread on the titanium substrate in situ, so that the porous titanium with a porous structure is prepared by Ag-Ti vacuum in situ hot melting reaction, and the principle is utilized as follows: ag is rapidly spread on a TA2 substrate, a layer of ultrathin Ag film is formed on the surface of the substrate, and simultaneously Ag is completely dissolved and diffused into a matrix and interacts with the TA2 substrate to promote the phase change of the matrix alpha-Ti to beta-Ti, so that the Ag is completely dissolved into the beta-Ti, and finally a porous structure with a micro-nano scale is formed; meanwhile, because the solubility of Ag in alpha-Ti and beta-Ti is different, redundant Ag can be separated out to form nano Ag particles in the phase change of the beta-Ti to the alpha-Ti in the cooling process. The porous structure formed by the porous titanium reduces the elastic modulus of the titanium, so that the elastic modulus of the titanium is matched with that of the bone under a certain condition, and the porous titanium also has the mechanical property similar to that of the bone and a unique porous structure; the Ag film spread on the substrate can be completely dissolved and diffused into the titanium matrix and can be separated out to form nano Ag particles in phase change, and the nano Ag particles can play a good role in sterilization in biomedical application; the porous titanium integral structure prepared by the invention has good comprehensive biomedical performance, and can be particularly applied to artificial teeth, bones and joint systems.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a scanning electron micrograph of porous titanium prepared in example 1;
FIG. 2 is an EDS surface scan energy spectrum of porous titanium prepared in example 1;
FIG. 3 is a transmission electron microscope image of porous titanium prepared in example 1;
in fig. 3, 1-nano silver particles.
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.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
A preparation method of porous titanium based on vacuum in-situ hot melting reaction comprises the following specific steps:
selecting a TA2 pure titanium metal plate with a smooth surface, and grinding and polishing the pure titanium metal plate to manufacture a sheet-shaped substrate with the size of 10mm multiplied by 0.5 mm; placing a silver sheet with the diameter of 5mm and the thickness of 100 mu m at the center of the prepared TA2 pure titanium substrate; the mixture is placed in a heating furnace for heating, and the heating is carried out under vacuum. Heating temperature is 1000 ℃, and heat preservation is carried out for 1min, so as to obtain a final spreading sample, namely the porous titanium.
The front and side surfaces of the porous titanium are analyzed by a Scanning Electron Microscope (SEM) and an energy spectrum (EDS), and the scanning electron microscope images are shown in figures 1 and 2, so that the result shows that a porous structure is obtained, the average size of finally measured pores is about 5-10 microns, and the depth of the porous structure is 20 microns. The surface area of titanium can be increased by the porous structure, and the elastic modulus is reduced to 75GPa through the determination of a nano-indenter, so that the biocompatibility of the titanium is improved; fig. 3 shows that the nano-Ag particles precipitated in the porous structure can be observed, and the nano-Ag particles precipitated in the porous structure can play a good role in sterilization; the porous titanium has uniform pore distribution and controllable size arrangement, can be applied to titanium filter core materials and medical porous titanium materials, and particularly can be applied to artificial teeth, bones and joint systems.
Example 2
The difference from the example 1 is that the heating temperature of the example 2 is 1020 ℃, the holding time is 2min, and other conditions are the same as the example 1.
Also, in example 2, a porous structure was obtained, but the size and depth of the pores were varied, and the average size of the pores was found to be about 10 to 20 μm and the depth of the porous structure was found to be 49 μm. Compared with the embodiment 1, the size of the pore is increased, the depth of the porous structure is increased, and the elastic modulus is reduced to 60GPa through the measurement of a nano-indenter, so that the biocompatibility is improved; the nano Ag particles precipitated in the porous structure can play a good role in sterilization; the porous titanium has uniform pore distribution and controllable size arrangement, can be applied to titanium filter core materials and medical porous titanium materials, and particularly can be applied to artificial teeth, bones and joint systems.
Example 3
The difference from the example 1 is that the heating temperature of the example 3 is 1030 ℃, the holding time is 3min, and other conditions are the same as the example 1.
Also, in example 3, a porous structure was obtained, but the size and depth of the pores were varied, and the average size of the pores was found to be about 15 to 30 μm and the depth of the porous structure was found to be 72 μm. Compared with the embodiment 1 and the embodiment 2, the size of the pore is increased, the depth of the porous structure is increased, and the elastic modulus is reduced to 52GPa through the measurement of a nano-indenter, so that the biocompatibility is improved; the nano Ag particles precipitated in the porous structure can play a good role in sterilization; the porous titanium has uniform pore distribution and controllable size arrangement, can be applied to titanium filter core materials and medical porous titanium materials, and particularly can be applied to artificial teeth, bones and joint systems.
Example 4
The difference from example 1 is that the heating temperature of example 4 is 1040 ℃, the holding time is 4min, and other experimental conditions are the same as example 1.
Example 4 also yielded a porous structure, but the size and depth of the pores varied, and the average size of the pores was found to be about 15 to 40 μm, with the depth of the porous structure being 96 μm. Compared with the embodiment 1, the size of the pore is increased, the depth of the porous structure is increased, and the elastic modulus is reduced to 40GPa through the measurement of a nano-indenter, so that the biocompatibility is improved; the nano Ag particles precipitated in the porous structure can play a good role in sterilization; the porous titanium has uniform pore distribution and controllable size arrangement, can be applied to titanium filter core materials and medical porous titanium materials, and particularly can be applied to artificial teeth, bones and joint systems.
Heating in a heating furnace, raising the temperature to melt and spread Ag to form an ultrathin Ag film, accelerating the hot melting reaction of the Ag film, enabling the in-situ reaction between Ag and Ti to be stronger when the temperature is higher, and increasing the temperature to form a porous structure with larger size.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (7)

1. A preparation method of porous titanium based on vacuum in-situ hot melting reaction is characterized by comprising the following steps:
(1) pretreating a pure titanium metal plate to obtain a TA2 substrate;
(2) placing a pure silver sheet in the center of a prepared TA2 substrate, heating the pure silver sheet in a vacuum environment to melt and spread Ag on a TA2 substrate, forming an Ag film on the surface of the substrate, and completely dissolving and diffusing the Ag film spread on the substrate into a titanium matrix to realize in-situ reaction between silver and titanium, thereby obtaining porous titanium;
the TA2 substrate is a sheet substrate;
the TA2 substrate has the size of 10mm multiplied by 0.5 mm; the pure silver sheet is circular, the diameter of the pure silver sheet is 5mm, and the thickness of the pure silver sheet is 100 mu m.
2. The vacuum in-situ hot melt reaction-based porous titanium preparation method as claimed in claim 1, wherein the pretreatment of the pure titanium metal plate comprises cutting, grinding and polishing.
3. The method for preparing porous titanium based on vacuum in-situ hot melting reaction according to claim 1, wherein the vacuum degree of the vacuum environment is 1E-4 ~5E -5 Pa。
4. The preparation method of porous titanium based on vacuum in-situ hot melting reaction according to claim 1, wherein the heating temperature is 1000-1050 ℃, and the holding time is 1-4 min.
5. The porous titanium prepared by the preparation method of the porous titanium based on the vacuum in-situ hot melting reaction according to any one of claims 1 to 4.
6. Use of the porous titanium of claim 5 in biomedicine.
7. Use of porous titanium in biomedicine according to claim 6, characterised in that it is the use of porous titanium in artificial teeth, bones and joint systems.
CN201910734381.9A 2019-08-09 2019-08-09 Porous titanium based on vacuum in-situ hot melting reaction, preparation method and application thereof Active CN110343894B (en)

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JP2006083444A (en) * 2004-09-17 2006-03-30 National Institute For Materials Science Porous titanium alloy
US9481036B2 (en) * 2011-12-09 2016-11-01 The Curators Of The University Of Missouri Method for fabricating biocompatible porous titanium
CN105435305B (en) * 2015-12-17 2019-02-26 西南交通大学 A kind of POROUS TITANIUM composite material and preparation method
CN107523711A (en) * 2016-06-21 2017-12-29 张家港市思杰五金工具有限公司 The preparation method of POROUS TITANIUM silver alloy
CN106552940B (en) * 2016-10-17 2018-05-25 昆明理工大学 A kind of preparation method of the ordered porous TiAg alloys of gradient
CN109622958B (en) * 2018-12-20 2020-06-02 华中科技大学 Method for preparing titanium alloy implant by adopting minimum curved surface porous structure

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