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WO2021113999A1 - Mousse d'alliage à base de titane ; procédé de préparation dudit alliagge ; et son utilisation comme biomatériau - Google Patents

Mousse d'alliage à base de titane ; procédé de préparation dudit alliagge ; et son utilisation comme biomatériau Download PDF

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Publication number
WO2021113999A1
WO2021113999A1 PCT/CL2019/050140 CL2019050140W WO2021113999A1 WO 2021113999 A1 WO2021113999 A1 WO 2021113999A1 CL 2019050140 W CL2019050140 W CL 2019050140W WO 2021113999 A1 WO2021113999 A1 WO 2021113999A1
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Prior art keywords
titanium
alloy
porosity
alloys
based alloy
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Ceased
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English (en)
Spanish (es)
Inventor
Claudio AGUILAR RAMÍREZ
Christopher Gonzalo SALVO MEDALLA
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Universidad Tecnica Federico Santa Maria USM
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Universidad Tecnica Federico Santa Maria USM
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Anticipated expiration legal-status Critical
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Classifications

    • 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
    • A61L27/06—Titanium or titanium alloys
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/08—Alloys with open or closed pores
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium

Definitions

  • the present invention relates to titanium-based alloy foams, their preparation method and their use as a biomaterial in biomedical applications.
  • the aging of the population constitutes one of the most relevant social and demographic events in recent decades, characterized by the increase in people who are 60 years of age or older. Its relevance is due to the fact that this process has multiple impacts on society, not only in the fields of education and health, but also in the economy and in the composition of the workforce.
  • Biomaterials may be suitable to solve these problems (serve as implants), it is expected that these biomaterials exhibit appropriate properties such as: excellent resistance to corrosion in the body fluid medium, mechanical and fatigue resistance, low modulus of elasticity, low density and good wear resistance, and stay in service longer without failure.
  • Stainless steel, Co-based alloys, Co-Cr and Ti-6AI-4V alloys are used as implants under load conditions (Xiong, J., et al., “Mechanical properties and bioactive surface modification via alkali-heat treatment of a porous Ti-18Nb-4Sn alloy for biomedical applications. "Acta Biomater., 2008. 4 (6): p. 1963-1968; Aguilar, C., et al.,” Synthesis and characterization of Ti-Ta- Nb- Mn foams. Materials Science and Engineering ” ⁇ . C, 2016. 58: p. 420-431).
  • Ti and its alloys have interesting properties that include high mechanical strength, lightness, excellent resistance to oxidation, and high biocompatibility. Compared with stainless steel, alloys based on cobalt (Co-Cr), Ti and alloys based on Ti have better biocompatibility, corrosion resistance and a lower elastic modulus (Long M. and HJ Rack, “Titanium alloys in total joint replacement — a materials Science perspective. ”Biomaterials, 1998. 19 (18): p. 1621-1639), so its use as a biomaterial has increased.
  • Ti-6AI-4V was the first a + by microstructure alloy that is widely used today as a biomaterial.
  • V and Al ions can be released into the human body, increasing the likelihood of disease.
  • V ions are released into human tissues, the kinetics of enzyme activity associated with inflammatory response cells are altered, and Al ions increase the likelihood of developing Alzheimer's.
  • materials scientists are investigating the alloy of non-toxic elements to produce new Ti-based alloys that meet the properties required for biomaterials.
  • the alloying elements tested are: Nb, Ta, Mo, Ta, Mn.
  • the alloying elements that have a different biological impact, so the best candidates to be considered biocompatible are: Ta, Nb, Zr, Au, Sn, Ru and Mn.
  • the most promising alloying elements for synthesizing Ti-based alloys are the 3d, 4d and 5d transition metals.
  • Ti-based alloys with a + b microstructure have been obtained using alloying elements such as Nb and Fe, but the elastic modulus values are higher (more than 100 GPa) compared to the elastic modulus of human bones, between 4 and 30 GPa for cortical bones and between 0.01 and 2 GPa for human cancellous bone. If the orthopedic implant has a higher elastic modulus value than human bone, the phenomenon called stress shielding occurs, which causes a high resorption rate.
  • metallic foams are defined as a mixture of metallic structure with embedded pores (open and / or closed), and present mixed properties between metals and foams.
  • Metallic foams possess a unique combination of properties, such as their low density, permeability to air and water, ability to absorb impact energy, low thermal conductivity, and good electrical insulation.
  • the main disadvantage of foams is that their elastic limit decreases as porosity increases.
  • biomaterial that shows properties such as high biocompatibility, low density, high mechanical strength and fatigue resistance, low elastic modulus and good wear resistance. More particularly, it is desirable that the biomaterial has a Young's modulus that matches the surrounding bone, and that in turn is strong and durable enough to withstand the physiological loads that have been applied to it over the years. Therefore, it is required to find a material that presents a suitable balance between strength and stiffness to better match the behavior of the bone.
  • the present invention discloses Ti-based alloy foams with elastic moduli less than 30 GPa and an elastic limit greater than 200 MPa.
  • Figure 1 General diagram of the Powder Metallurgy process.
  • Figure 2 Microstructures in titanium alloys.
  • FIG. 3 Titanium binary alloys.
  • Figure 4 Modulus of elasticity for various alloys.
  • Figure 5 Photograph of a glove box.
  • Figure 6 Schematic and photograph of a planetary mill.
  • Figure 8 Photograph of a Compaction system.
  • Figure 9 Photograph of the equipment used in sintering.
  • Figure 10 SEM images of mechanically alloyed powders.
  • FIG. 11 EDS of mechanically alloyed powders.
  • Figure 12 Diffractogram of the Ti-13Ta-12Sn alloy (% at.)
  • Figure 14 SMEB images at 200X magnification of samples with bimodal microstructure.
  • Figure 15 Graph of apparent porosity as a function of theoretical porosity.
  • Figure 16 Graph of Density measured as a function of porosity.
  • Figure 17 Graph of the Modulus of elasticity measured as a function of porosity.
  • Figure 18 Graph of yield stress measured as a function of porosity.
  • cellular metals and "metallic foams” are used to refer to metals and alloys whose structure is porous.
  • cellular metals is used when the metal exhibits porous foams and the term metallic foams is used when a synthesis process is applied to obtain foams.
  • Metal foams with open pores can be obtained through solid, liquid or gaseous phases and the selection of the method depends on the type, distribution and size of the pores.
  • a simple solid state process to obtain foams with a distribution of pores and type of porosity (open and closed pores) is the "spacers" method. This method allows to control the shape, size and distribution of porosity through sintering temperature, time and dissolution temperature (if the spacer is salt). Spacers commonly used to synthesize Ti foams are: carbamide, ammonium hydrogen carbonate (NFI4FICO3), tapioca starch, salt (NaCl), magnesium, ACRAWAX® (AW), PMMA, sucrose and urea.
  • spacers commonly used to synthesize Ti foams are: carbamide, ammonium hydrogen carbonate (NFI4FICO3), tapioca starch, salt (NaCl), magnesium, ACRAWAX® (AW), PMMA, sucrose and urea.
  • the spacer should be selected based on the following criteria: i) size and shape, ii) cost, iii) reactivity of the Ti with the support, iv) presence of left residues, v) easy processability and vi) non-toxic element.
  • the residues In the case of biomedical foams, the residues must be bio-inert or biocompatible, that is, in the case of ammonium hydrogen carbonate, urea and tapioca starch, the human body can absorb residues that could cause some problems.
  • the NaCI particles have the advantage that their residues do not cause problems to the human body (they are not toxic) and they are easily removable by the process of dissolution in water.
  • ammonium bicarbonate as a spacer material has the advantages of not reacting with titanium during the process and is eliminated by the contribution of heat during sintering, due to its decomposition when subjected to a temperature above 35oC, producing ammonia vapors according to the reaction:
  • the porosity resulting from the preparation method and the mechanical properties obtained for the foams are highly dependent on the particle mixture of the support of the metal powder space.
  • Powder metallurgy or powder metallurgy is a manufacturing process that takes metallic powders with certain characteristics such as size, shape and packaging to create a figure of high hardness and precision.
  • One of the advantages of Powder Metallurgy is the ability to manufacture parts with complex shapes and dimensions close to those of the final product, with excellent tolerances, high quality and at a relatively low cost, that is, parts are obtained with greater homogeneity and control of the size of the grains, achieving the formation of strong bonds between the particles and, therefore, increases in the hardness and toughness of the materials.
  • This process is suitable for the manufacture of large series of small parts with great precision, for pure materials or unusual mixtures and to control the degree of porosity or permeability, in addition there is a reduction in costs due to the possibility of eliminating the processes of finishing, compared to other manufacturing methods such as forging or casting.
  • Figure 1 shows a general diagram of the stages of the basic powder metallurgy process.
  • the manufacture of PM components begins with the mixing of powders, additives and lubricants. This mixture is compacted as a piece inside a mold that has the desired shape, by applying pressure. After compaction, the mixture takes on the properties of a solid, whose state is called "green". Subsequently, the compact is sintered to temperatures below the melting point, under a controlled atmosphere, achieving a metallurgical bond between the particles.
  • the basic operations of compacting and heating can be combined in various ways in processes for the manufacture of metal powders.
  • alloying elements to pure titanium produce a range of possible microstructures in titanium alloys. That is, the addition of other elements to titanium can be obtained: Alpha alloys (a), Alpha-beta alloys (a-b) and beta alloys (b). These alloys are characterized by the phases (crystalline structures) that exist in the alloy when they are close to room temperature and possess different properties as shown in Figure 2. The temperatures at which the alpha and beta phases can exist are they alter as alloying elements are added to the titanium. Depending on their influence on the proportions of the alpha and beta phases below the beta trans, the alloying elements are divided into three groups:
  • Beta stabilizers stabilizes the beta phase at lower temperatures
  • Alpha (a) Alloys are characterized by their strength, toughness, yield stress and weldability.
  • Alpha stabilizing solutes are those that, as a function of concentration, raise the temperature of the (a + b) / a transus.
  • Such solutes are generally not transition metals (ie "simple metals", SM).
  • Beta alloys In the case of Beta Alloys (b), the transition solutes (metal) are stabilizers of the bcc phase. Therefore, all b-alloys generally contain large amounts of one or more of the so-called “b-isomorphs” forming additions: vanadium, niobium, tantalum (group V transition metals) and molybdenum (group VI transition metals). Beta alloys are metastable; that is, they tend to transform into a balance or balance of structures. The Beta alloys generate strength from the intrinsic strength of the beta structure and the precipitation of the alpha and other phases of the alloy through heat treatment after processing.
  • beta structure The most significant benefit provided by a beta structure is the increased formability of such alloys relative to the hexagonal crystal structure types (alpha and alpha-beta).
  • Formability can be defined as a measure of the amount of deformation that a material can undergo in a forming process without failure, such as localized thinning or fracture.
  • Other characteristics of beta alloy are: being heat treatable at high strength levels, excellent tensile strength up to 370 ° C, low creep resistance above 370 ° C, good solderability as solution treated, good toughness, slow rate fatigue crack growth and contains sufficient beta stabilizer to retain a fully beta structure at room temperature, which increases ductility.
  • the alloys a + b are such that, in equilibrium, generally at room temperature, they admit a mixture of phases a and b. Although many stabilized binary alloys b in thermodynamic equilibrium are two-phase, in practice alloys a + b generally contain mixtures of stabilizers a and b. A + b alloys generally exhibit good workability, as well as high room temperature strength and moderate elevated temperature strength. They can contain between 10 and 50% phase b at room temperature; if they contain more than 20%, they are not weldable. The properties of alloys a + b can be controlled by heat treatment, which is used to adjust the microstructural states and precipitation of component b. The alloys are formulated so that both the alpha phase (hcp) and the beta phase (bcc) exist at room temperature. These alloys, to some extent, compromise some of the characteristics of alpha and beta alloys.
  • the titanium-based alloy foam is Ti-13Ta-3Sn.
  • the titanium-based alloy foam is Ti-13Ta-6Sn.
  • the titanium-based alloy foam is Ti-13Ta-12Sn.
  • the titanium-based alloy foam has a porosity of up to 50%.
  • the titanium-based alloy foam has an elastic modulus of up to 30 GPa.
  • the titanium-based alloy foam has an elastic limit greater than 200 MPa.
  • the alloy preparation step is carried out by mechanical alloying.
  • the step of preparing the green specimens is carried out by compacting the alloy.
  • the step of preparing the green specimens uses a spacer material.
  • the spacer material is ammonium bicarbonate.
  • the sintering step of the compacted green specimens is carried out in a tube furnace.
  • the sintering step is carried out at 1300 ° C.
  • the present invention is directed to the use of the titanium-based alloy foam as a biomaterial.
  • the biomaterial is a bone implant.
  • the Ti-13Ta-12Sn alloy was prepared by mechanical alloying (grinding), using titanium, tantalum and tin metal powders as raw material. What controlling agent of the mechanical alloying process (grinding), triple stearic acid (CH3 (CH2) i6COOH) was used at 2% by weight.
  • Ammonium bicarbonate (NH4HCO3) was used as spacer material ((NH4HCO3).
  • Zirconium oxide balls YSZ (YSZ stabilized ZrÜ2) were used as grinding medium. Balls of 5 and 10 mm in diameter were used, in a ratio in mass of balls with respect to the powder of 10: 1.
  • YSZ stabilized ZrÜ2 Two YSZ zirconium oxide vessels (YSZ stabilized ZrÜ2) were used for grinding the powders.
  • Zinc stearate was used as a solid lubricant in the compaction of the green specimen.
  • the alloyed powders were recovered.
  • the green test tubes were then prepared. At this stage the powders are compacted in the compaction machine.
  • Samples with a bimodal microstructure were obtained by mixing 25% of the weight of the ground powders with 75% of the weight of the raw powders.
  • the bimodal microstructure (+ BM) is defined as a mixture of 25% nanoparticles and 75% micrometric particles.
  • Samples without bimodal microstructure (-BM) were obtained with raw powders.
  • an amount of spacer material was added according to the percentage of porosity that was wanted to obtain in the test tubes (0%, 30%, 40% and 50%).
  • Table 2 shows the mass of each of the elements.
  • Sintering was carried out in a tube furnace (see Figure 9) using a controlled argon atmosphere.
  • the green specimens to be sintered were introduced.
  • the cycle has two isotherms, the first corresponds to the volatilization of the spacer material, which is carried out at 180 ° C for an hour and a half.
  • the second isotherm corresponds to the sintering of the metal alloy, which is carried out at 1,300 ° C for 3 h. After cooling, the specimens were removed from the oven.
  • the morphology of the powders and foams obtained were studied by scanning electron microscopy (SEM).
  • the porosity of the foams was measured using image analysis software obtained using an optical microscope coupled to a Leica MC170 HD camera.
  • the ultrasonic measurements of the elastic modulus were carried out using ultrasonic transducers.
  • the measurement and calculation protocol is based on the ASTM D2845-08 standard.
  • Density measurement was performed with a 20 ml pycnometer and a balance with a sensitivity of 0.001 g, based on the ASTM D792-08 standard. Compression tests were carried out with a Zwick-Roell machine at a loading speed of 0.02 mm / min according to BS ISO 14317: 2015.
  • Figure 10 shows SEM images of mechanically alloyed powders for 50 h at magnification of a) 1000X, b) 5000X, c) 7500X and d) 10000X of the titanium alloy (Ti-13% Ta-12% Sn (% at.)) .
  • An irregular morphology was observed, with some agglomerated particles, rounded edges and others scattered.
  • a not very homogeneous size distribution was observed, with the formation of a spherical morphology.
  • the cold welding and fracture processes coexist during the grinding process, however, there is the predominance of cold welding, since it was observed that the particles have a spherical morphology.
  • Figure 12 shows the X-ray diffraction patterns of the Ti-13Ta-12Sn (atomic%) alloy powders ground at different times. The formation of a new phase with fcc structure was observed as time passed and simultaneously the decrease of the beta phase with the passing of the hours. The highest amount of alpha titanium was reported at 5 h, then, over time, its amount decreased until 40 h, where this phase is no longer present.
  • the pore size distribution varies significantly, since it is possible to find pores with sizes from 40 prm to 770 miti, even small black dots are observed that correspond to formed micropores, this phenomenon is notably appreciated in the bulk of the sample with bimodal structure (0% porosity).
  • the shape of the pores is completely irregular, this can be explained by the geometric shape of the spacer material used (ammonium bicarbonate).
  • Figure 14 shows the representative images at 200X magnification of the samples with bimodal microstructure with a) 0% porosity, b) 30% porosity, c) 40% porosity and d) 50% porosity; and without bimodal microstructure with e) 0% porosity, f) 30% porosity, g) 40% porosity and h) 50% porosity.
  • the interconnection of the pores, the irregularity of their shape and their different size distribution are observed, as well as the existence of two different shades. Determination of Porosity
  • the apparent porosity is the ratio of the volume of the open pores of the sample with its external volume and does not consider the volume of the closed pores.
  • the increase in porosity can be explained not only by the porosity introduced by the spacer material, but also by that generated with the sintering itself between the particles, that is, micropores were formed that increase the percentage of porosity.
  • the porosity in foams with bimodal structure is slightly higher than those without bimodal microstructure, so it is possible to conclude that the addition of bimodal microstructure promotes the generation of interconnected porosity.
  • the modulus of elasticity was obtained through the ultrasound test, the results are shown in Table 4 and graphed in Figure 17.
  • An inverse linear relationship is obtained with respect to the theoretical porosity, that is, as the% porosity increases, decreases the modulus of elasticity. This relationship is to be expected, since the modulus of elasticity of a porous material decreases as the porosity increases.
  • the modules obtained in both structures are compared, it is possible to appreciate that in the case of the bimodal microstructure, lower values were obtained compared to without bimodal microstructure; however, as the% porosity increases, the difference between the two lines decreases, and where the modulus of elasticity is modified according to the% porosity.
  • the specimens with bimodal microstructure have a lower value of Young's modulus compared to the specimens without bimodal microstructure; however, as the% porosity increases, the difference between the two lines decreases.
  • the specimens that meet this value for implantation in the human body would correspond to foams with a porosity of 30%, 40% and 50% with and without bimodal microstructure.
  • Specimens with bimodal microstructure and porosity meet the mechanical requirements to serve as biomedical implants, elastic modulus less than 30 GPa and yield stress in compression over 120 MPa.

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  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dermatology (AREA)
  • Manufacturing & Machinery (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
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Abstract

La présente invention concerne une mousse d'alliage à bas de titane de formule Ti-13Ta-XSn, où X = 3, 6, 9 et 12 % atomiques. La mousse d'alliage à base de titane présente une porosité allant jusqu'à 50%, un module élastique allant jusqu'à 30GPa et une limite élastique supérieure à 200 MPa. L'invention concerne également un procédé de préparation de ladite mousse d'alliage à base de titane, et l'utilisation de celle-ci comme biomatériau, en particulier pour implants osseux.
PCT/CL2019/050140 2019-12-13 2019-12-13 Mousse d'alliage à base de titane ; procédé de préparation dudit alliagge ; et son utilisation comme biomatériau Ceased WO2021113999A1 (fr)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2459686C2 (ru) * 2010-07-15 2012-08-27 Государственное образовательное учреждение высшего профессионального образования Самарский государственный технический университет Способ получения пористых биосовместимых материалов на основе никелида титана
WO2018009582A1 (fr) * 2016-07-05 2018-01-11 Porosteon Development Llc Dispositifs métalliques poreux

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2459686C2 (ru) * 2010-07-15 2012-08-27 Государственное образовательное учреждение высшего профессионального образования Самарский государственный технический университет Способ получения пористых биосовместимых материалов на основе никелида титана
WO2018009582A1 (fr) * 2016-07-05 2018-01-11 Porosteon Development Llc Dispositifs métalliques poreux

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Title
AGUIRRE, T.: "Efecto De La Estructura Biomodal Y Porosidad Sobre EI Modulo De Elasticidad Y Esfuerzo De Fluencia En Espumas De Ti-Ta-Sn. Tesis de pregrado para optar al titulo de ingeniero civil metalúrgico", TESIS DE PREGRADO PARA OPTAR AL TITULO DE INGENIERO CIVIL METALÚRGICO, March 2018 (2018-03-01), Universidad Tecnica Federico Santa Maria, Chile, XP055834675, Retrieved from the Internet <URL:https://repositorio.usm.cl/bitstream/handle/11673/24077/3560900258117UTFSM.pdf?sequence=1&isAllowed=y> [retrieved on 20200417] *
ARNALDI, C. ET AL.: "Analysis Of Synthesis And Mechanical Properties Of Ti-Ta-Sn Foams For Use In Biomedical Applications", XXVII INTERNATIONAL MATERIALS RESEARCH CONGRESS, 2018 *
ARNALDI, C.: "Análisis De Sintesis Y Propiedades Mecanicas De Espumas Ti-Ta-Sn Para El Uso En Aplicaciones Biomedicas. Tesis de pregrado para optar al tituio de ingeniero civil metalurgico", TESIS DE PREGRADO PARA OPTAR AL TITULO DE INGENIERO CIVIL METALÚRGICO, September 2019 (2019-09-01), Universidad Tecnica Federico Santa Maria, Chile, XP055834676, Retrieved from the Internet <URL:https://repositorio.usm.cl/bitstream/handle/11673/47205/3560900260918UTFSM.pdf?sequence=1&isAllowed=y> [retrieved on 20200416] *
PALKA, K. ET AL.: "Porous Titanium Implants", ADVANCED ENGINEERING MATERIALS, vol. 20, no. 5, May 2018 (2018-05-01), pages 1700648, XP055834677, DOI: 10.1002/adem.201700648 *
XIONG LI, WONG JIANYU, HODGSON CYNTHIA S, PETER D, CUI WEN, LI YUNCANG, PH D, XIONG JIANYU, ENG M, WONG CYNTHIA S, PH D, HODGSO: "Ti6Ta4Sn Alloy and Subsequent Scaffolding for Bone Tissue Engineering", TISSUE ENGINEERING: PART A, vol. 15, no. 10, 1 October 2009 (2009-10-01), pages 3151 - 3159, XP055834678 *

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