CN116121588A - High-performance titanium alloy for artificial joint and preparation method thereof - Google Patents
High-performance titanium alloy for artificial joint and preparation method thereof Download PDFInfo
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 159
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000000956 alloy Substances 0.000 claims abstract description 57
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 51
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000005242 forging Methods 0.000 claims abstract description 14
- 238000003723 Smelting Methods 0.000 claims abstract description 12
- 238000005096 rolling process Methods 0.000 claims abstract description 12
- 239000010936 titanium Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 64
- 238000001816 cooling Methods 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000006104 solid solution Substances 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 13
- 229910000883 Ti6Al4V Inorganic materials 0.000 abstract description 11
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000032683 aging Effects 0.000 description 14
- 206010040844 Skin exfoliation Diseases 0.000 description 10
- 125000004122 cyclic group Chemical group 0.000 description 9
- 239000007943 implant Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 230000002035 prolonged effect Effects 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000005498 polishing Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0075—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for rods of limited length
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- 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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/24—Materials or treatment for tissue regeneration for joint reconstruction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present disclosure provides a high performance titanium alloy for artificial joints and a method for preparing the same, wherein the titanium alloy comprises the following chemical components: nb with the mass ratio of: (13-15 wt.%; mo, the mass ratio is: (5-6 wt.%; zr, the mass ratio is: (5-6 wt.%; the balance being Ti. The method comprises the following steps: according to the component proportion, raw materials are obtained and uniformly mixed; smelting the uniformly mixed raw materials in a vacuum consumable manner to prepare alloy ingots; forging and rolling the alloy cast ingot to obtain a rolled rod; peeling the surface of the rolled rod to obtain a blank; heat-treating the blank to obtain a titanium alloy bar blank; and (3) finishing the titanium alloy rod blank to obtain a titanium alloy rod, namely the high-performance titanium alloy for the artificial joint. According to the invention, the alloy composition proportion design of Nb (13-15 wt.%), mo (5-6 wt.%) and Zr (5-6 wt.%) is adopted, the prepared titanium alloy has high strength and low elastic modulus, the elastic modulus is half of that of titanium alloy Ti6Al4V, the elastic modulus is closer to that of human skeleton, shielding can be effectively avoided in the use process, and the use safety and service life are improved.
Description
Technical Field
The present disclosure relates to the technical field of artificial joint surgical implants, and in particular to a high-performance titanium alloy for an artificial joint and a preparation method thereof.
Background
The artificial joint is mainly used for joint replacement of hip, knee, shoulder and other parts of a human body in the field of surgical implants, bears large stress in the clinical application process, has high requirements on the comprehensive performance of joint materials, and has high strength, high toughness and good wear resistance. Meanwhile, the material can be separated from the instrument part by metal fragments due to friction characteristics and fused in human tissues, so that the biocompatibility of the material is particularly important. In addition, the artificial joint is used in a human body for a long time, and the stress shielding can be caused due to the problem of matching degree of stress action and skeleton elastic modulus, so that the artificial joint is shifted and fails.
At present, titanium alloy materials, namely pure titanium 4A and titanium alloy Ti6Al4V, for example, patent No. CN103436831B, are widely applied, and a preparation method of a titanium alloy bar for surgical implants is disclosed, wherein the preparation method comprises the steps of blank preparation, cogging forging, deformation processing, annealing processing, hot straightening, finishing processing and secondary polishing. The preparation method of the titanium alloy bar for the surgical implant improves the quality and the performance of the titanium alloy bar after three-time straight and three-time annealing treatment, meets the requirement of an outlet, and in addition, the invention heats and keeps the titanium alloy ingot at the temperature, uses hammering equipment to enable the deformation rate to reach 50-60 percent, then performs upsetting and drawing for 6-9 times, improves the compactness of the titanium alloy, and ensures the performance and the metallographic structure of the titanium alloy bar by adopting the temperature which is lower than 970 ℃ of the phase transition point of the titanium alloy in intermediate forging and rolling finished products.
It can be seen that the titanium alloy ingots meeting the requirements of GB/T13810-2017 standard are still adopted as blanks in the prior art, but the titanium alloys have the problems of lower strength, existence of elements which are not attached to the human tissue environment and poor matching with the skeleton elastic modulus in combination with the application characteristics and requirements of joints although the cost is lower and the processing and manufacturing process is mature. Therefore, a titanium alloy material with high strength, low elastic modulus and excellent biocompatibility can be developed, the use safety of the joint can be remarkably improved, and the service life can be prolonged.
It should be noted that the information disclosed in the above background section is only for enhancing understanding of the background of the present disclosure and thus may include information that does not constitute prior art known to those of ordinary skill in the art.
Disclosure of Invention
The present disclosure is directed to a high-performance titanium alloy for an artificial joint and a method for producing the same, and further, it is desired to develop a titanium alloy material that can obtain high strength, low elastic modulus, and excellent biocompatibility.
Other features and advantages of the present disclosure will be apparent from the following detailed description, or may be learned in part by the practice of the disclosure.
According to a first aspect of the present disclosure, there is provided a high-performance titanium alloy for an artificial joint, comprising, in mass percent:
nb with the mass ratio of: (13-15 wt.%;
mo, the mass ratio is: (5-6 wt.%;
zr, the mass ratio is: (5-6 wt.%;
the balance being Ti.
According to a second aspect of the present disclosure, there is provided a method for preparing a high-performance titanium alloy for an artificial joint, comprising:
according to the component proportion, raw materials are obtained and uniformly mixed;
smelting the uniformly mixed raw materials in a vacuum consumable manner to prepare alloy ingots;
forging and rolling the alloy cast ingot to obtain a rolled rod;
peeling the surface of the rolled rod to obtain a blank;
heat treating the blank to obtain a titanium alloy bar blank;
and (3) finishing the titanium alloy rod blank to obtain a titanium alloy rod, namely the high-performance titanium alloy for the artificial joint.
Optionally, the step of heat treating the billet to obtain a titanium alloy bar billet comprises:
carrying out solid solution treatment on the blank;
and heating, preserving heat and cooling the blank subjected to the solution treatment, and circulating for a plurality of times to obtain a titanium alloy bar blank.
Optionally, the step of solution treating the blank comprises:
heating the blank to 820 ℃, and preserving heat for 90 minutes;
cooling the blank after heat preservation in flowing water to a room temperature state;
transferring the blank cooled to the room temperature state into liquid nitrogen for cryogenic treatment to obtain the blank after solution treatment.
Optionally, the step of heating, preserving heat and cooling the blank after solution treatment and circulating for a plurality of times to obtain a titanium alloy bar blank comprises:
heating for the first time, heating the blank subjected to solution treatment to 520 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way;
heating for the second time, heating the blank subjected to the first heating treatment to 460 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way; obtaining the titanium alloy rod blank.
Optionally, performing the first heating and the second heating at least once in sequence to obtain the titanium alloy rod blank.
Optionally, the steps of obtaining raw materials and mixing uniformly:
nb is added in the form of NbTi intermediate alloy, mo is added in the form of TiMo intermediate alloy, zr is added in the form of sponge zirconium, and the balance is sponge titanium.
Optionally, the step of vacuum consumable smelting the uniformly mixed raw materials to prepare the alloy ingot comprises the following steps:
preparing the uniformly mixed raw materials into an electrode;
carrying out vacuum consumable smelting on the electrode to obtain an alloy cast ingot;
wherein the alloy ingot has a diameter phi of 600mm and a single weight of about 3000kg.
Optionally, forging and rolling the alloy ingot to obtain a rolled rod, wherein the diameter phi of the rolled rod is 55-95mm.
Optionally, the diameter of the titanium alloy rod is phi 50-90mm.
The present disclosure provides a high performance titanium alloy for artificial joints and a method for preparing the same, wherein the titanium alloy comprises the following chemical components: nb with the mass ratio of: (13-15 wt.%; mo, the mass ratio is: (5-6 wt.%; zr, the mass ratio is: (5-6 wt.%; the balance being Ti. The method comprises the following steps: according to the component proportion, raw materials are obtained and uniformly mixed; smelting the uniformly mixed raw materials in a vacuum consumable manner to prepare alloy ingots; forging and rolling the alloy cast ingot to obtain a rolled rod; peeling the surface of the rolled rod to obtain a blank; heat-treating the blank to obtain a titanium alloy bar blank; and (3) finishing the titanium alloy rod blank to obtain a titanium alloy rod, namely the high-performance titanium alloy for the artificial joint. According to the invention, the alloy composition proportion design of Nb (13-15 wt.%), mo (5-6 wt.%) and Zr (5-6 wt.%) is adopted, the prepared titanium alloy has high strength and low elastic modulus, the elastic modulus is half of that of titanium alloy Ti6Al4V, the elastic modulus is closer to that of human skeleton, shielding can be effectively avoided in the use process, and the use safety and service life are improved.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the disclosure and together with the description, serve to explain the principles of the disclosure. It will be apparent to those of ordinary skill in the art that the drawings in the following description are merely examples of the disclosure and that other drawings may be derived from them without undue effort.
Fig. 1 schematically illustrates a schematic diagram of a heat treatment process for a ti14.1nb5.6mo5.2zr titanium alloy in an exemplary embodiment of the disclosure.
Fig. 2 schematically illustrates a tissue topography of a solution treated blank in an exemplary embodiment of the present disclosure.
Fig. 3 schematically illustrates a schematic view of the structure morphology of the titanium alloy rod blank obtained by sequentially performing a first heating cycle and a second heating cycle in an exemplary embodiment of the present disclosure.
FIG. 4 schematically illustrates an exemplary embodiment of the present disclosure in which a first heating and a second heating cycle are sequentially performed to obtain a graphical representation of the structure morphology of the titanium alloy rod blank.
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. However, the exemplary embodiments may be embodied in many forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of the example embodiments to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Titanium alloy ingots meeting the requirements of GB/T13810-2017 standard are still adopted as blanks in the prior art, but the titanium alloys are low in cost, mature in processing and manufacturing process, and have the problems of low strength, existence of elements which are not attached to the human tissue environment and poor matching with the skeleton elastic modulus in combination with the application characteristics and requirements of joints. Therefore, a titanium alloy material with high strength, low elastic modulus and excellent biocompatibility can be developed, the use safety of the joint can be remarkably improved, and the service life can be prolonged.
In order to solve the problem, a technical scheme of the application is provided, which is specifically as follows:
example 1
According to a first aspect of the present disclosure, there is provided a high-performance titanium alloy for an artificial joint, comprising, in mass percent: nb with the mass ratio of: (13-15 wt.%; mo, the mass ratio is: (5-6 wt.%; zr, the mass ratio is: (5-6 wt.%; the balance being Ti.
In the present exemplary embodiment, in the process of actually obtaining the raw material of the high-performance titanium alloy for preparing the artificial joint, nb may be added in the form of NbTi intermediate alloy, mo may be added in the form of TiMo intermediate alloy, zr may be added in the form of zirconium sponge, and the rest of the components may be supplemented with titanium sponge, and it should be noted that the ratio of the above components needs to be ensured in the process of collocating the selected raw materials.
In the embodiment, the method adopts the design of the proportion of Nb= (13-15) wt.%, mo= (5-6) wt.%, and Zr= (5-6) wt.% alloying components, the prepared titanium alloy has low elastic modulus, the elastic modulus is half of that of the titanium alloy Ti6Al4V, the elastic modulus is closer to that of human skeleton, shielding can be effectively avoided in the use process, and the use safety and service life are improved.
According to a second aspect of the present disclosure, there is provided a method for preparing a high-performance titanium alloy for an artificial joint, comprising: step S110 to step S160.
S110, obtaining raw materials according to the component proportions and uniformly mixing.
Specifically, nb is added in the form of NbTi intermediate alloy, mo is added in the form of TiMo intermediate alloy, zr is added in the form of sponge zirconium, and the balance is sponge titanium, and the raw materials are weighed according to the proportion and mixed uniformly.
S120, smelting the uniformly mixed raw materials in a vacuum consumable manner to obtain alloy ingots.
Specifically, the electrode is manufactured by using the uniformly mixed raw materials as raw materials, and vacuum consumable smelting is adopted for three times to obtain an alloy ingot, and as a preferred embodiment, the ingot shape diameter of the alloy ingot can be phi 600mm, of course, the alloy ingot can also be of other sizes, a specific operator can determine the alloy ingot according to actual processing requirements, the single weight of the alloy ingot can be 3000kg, of course, the single weight of the alloy ingot can also be other weight, and the specific operator can determine the alloy ingot according to actual processing requirements.
And S130, forging and rolling the alloy cast ingot to obtain a rolled rod.
Specifically, the alloy ingot can be forged and rolled to obtain a rolled rod with a diameter phi of 55-95mm, in this embodiment, the forging He Gazhi can be an existing forging machine and rolling machine, and it is understood that the forging and rolling are used for making the uniformity of the alloy ingot better and making the rolled rod with a target diameter, wherein the target diameter can be the diameter phi of 55-95mm, can be other diameters, and can be determined by an operator according to actual production and processing requirements.
And S140, peeling the surface of the rolled rod to obtain a blank.
Specifically, the peeling of the surface of the rolled rod can be realized by selecting an existing peeling machine, the application is not limited to the type and model of the peeling machine, the working parameters of the peeling machine can be correspondingly adjusted according to the actual diameter of the rolled rod by a person skilled in the art, the specific parameter adjusting process is not limited, and the application needs to be interpreted that in the application, after the peeling treatment of the rolled rod, a blank can be obtained, and the blank is the raw material in the heat treatment process.
And S150, performing heat treatment on the blank to obtain a titanium alloy bar blank.
Specifically, the heat treatment process may include: the solid solution heat treatment and the cyclic aging heat treatment, specifically, the solid solution heat treatment can be to heat the blank to 820 ℃, keep the temperature for 90 minutes, quickly put into flowing water to be cooled after reaching the temperature, cooled to the room temperature state, and then quickly transferred into liquid nitrogen to be subjected to the cryogenic treatment. The morphology of the solution heat treated blank is shown in fig. 2.
The cyclic aging heat treatment can be to the blank after liquid nitrogen treatment, reheat to 520 ℃, keep the temperature for 2 hours, cool down to room temperature in the air, reheat to 460 ℃, keep the temperature for 2 hours, cool down to room temperature in the air, the above two steps heat treatment, can circulate many times.
Illustrating: the solution heat treatment is carried out to obtain a titanium alloy bar blank 1, and the cyclic aging heat treatment is carried out on the titanium alloy bar blank 1, wherein the following steps are carried out:
heating the titanium alloy rod blank to 1-520 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way; heating the titanium alloy rod blank cooled to room temperature to 460 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way; completing the first circulation to obtain a titanium alloy rod blank 1 after the first circulation; the structure morphology diagram of the titanium alloy rod blank 1 after one cycle is shown in fig. 3.
Heating the titanium alloy rod blank after one-time circulation to 1-520 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way; heating the titanium alloy rod blank cooled to room temperature to 460 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way; completing the second circulation to obtain a titanium alloy rod blank 1 after the second circulation; the structure morphology diagram of the titanium alloy rod blank 1 after the secondary circulation is shown in fig. 4.
The third cycle, the fourth cycle, etc. may be performed subsequently, and the number of cycles is not limited in this application, and it is to be understood that in this application, only the titanium alloy rod blank 1 after the first cycle may be used as the titanium alloy rod blank described in this application, or the titanium alloy rod blank 2 after the two cycles may be used as the titanium alloy rod blank described in this application, or the titanium alloy rod blank n after the n cycles may be used as the titanium alloy rod blank described in this application. It can be seen that the important point to be protected in this application is: the solution heat treatment and the cyclic aging heat treatment processes adopted in the application are not the number of times of circulation in the cyclic aging heat treatment process.
And S160, finely processing the titanium alloy rod blank to obtain a titanium alloy rod, wherein the titanium alloy rod is the high-performance titanium alloy for the artificial joint.
Specifically: and (3) carrying out finishing machining on the titanium alloy rod blank subjected to heat treatment to obtain a titanium alloy rod with the diameter of 50-90mm, wherein the titanium alloy rod is the high-performance titanium alloy for the artificial joint to be prepared in the application, and an operator can adopt the high-performance titanium alloy for the artificial joint as a raw material of a surgical implant.
It can be understood that in the present application, a method for manufacturing a titanium alloy rod with a finished product diameter of Φ50-90mm is exemplified, and a person skilled in the art can set the size of the finished product according to the size of the actual finished product, and the size of the finished product is not limited in the preparation process of step S110-step S160 of the present application, and any titanium alloy rod with other diameter manufactured by using the preparation process of the present application belongs to the protection scope of the present application.
In the embodiment, the specific cyclic heat treatment technology is adopted, the liquid nitrogen subjected to solution treatment is subjected to deep cooling to obtain a full beta phase structure, then the beta-alpha+beta phase transformation occurs through multi-stage aging treatment, the fine needle-shaped alpha+beta phase is separated out from a beta matrix, and the more the cyclic times are, the more the content of the fine needle-shaped alpha+beta phase is separated out, so that the titanium alloy has the characteristics of high strength and high toughness. The mechanical property of the material exceeds that of the conventional titanium alloy Ti6Al4V and the like, so that the fatigue fracture resistance of the material is further improved. It can be seen that: the invention combines biocompatibility and mechanical compatibility by reasonable alloying design and adopting specific heat treatment technology, and is an ideal titanium alloy material for manufacturing artificial joints.
In one embodiment, the step of heat treating the billet to obtain a titanium alloy rod billet comprises: carrying out solid solution treatment on the blank; and heating, preserving heat and cooling the blank subjected to the solution treatment, and circulating for a plurality of times to obtain a titanium alloy bar blank.
In one embodiment, the step of solution treating the blank comprises: heating the blank to 820 ℃, and preserving heat for 90 minutes; cooling the blank after heat preservation in flowing water to a room temperature state; transferring the blank cooled to the room temperature state into liquid nitrogen for cryogenic treatment to obtain the blank after solution treatment.
In one specific embodiment, the step of heating, preserving heat and cooling the blank after solution treatment and circulating for a plurality of times to obtain a titanium alloy bar blank comprises: heating for the first time, heating the blank subjected to solution treatment to 520 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way; heating for the second time, heating the blank subjected to the first heating treatment to 460 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way; obtaining the titanium alloy rod blank.
In a specific embodiment, the first heating and the second heating are sequentially performed at least once to obtain the titanium alloy rod blank.
In one embodiment, the steps of obtaining the raw materials and mixing are as follows: nb is added in the form of NbTi intermediate alloy, mo is added in the form of TiMo intermediate alloy, zr is added in the form of sponge zirconium, and the balance is sponge titanium.
In one specific embodiment, the step of vacuum consumable melting the uniformly mixed raw materials to produce an alloy ingot comprises: preparing the uniformly mixed raw materials into an electrode; carrying out vacuum consumable smelting on the electrode to obtain an alloy cast ingot; wherein the alloy ingot has a diameter phi of 600mm and a single weight of about 3000kg.
In a specific embodiment, the steps forge and roll the alloy ingot to obtain a rolled rod, wherein the diameter phi of the rolled rod is 55-95mm.
In one embodiment, the titanium alloy rod has a diameter of from Φ50mm to 90mm.
Example 2
On the basis of the embodiment 1, taking the manufacturing of a titanium alloy rod with the diameter of phi 50 as an example, the technical scheme of the application is further described in detail, and the method comprises the following steps of:
1. alloy design: the chemical components of the titanium alloy are as follows: nb= (13-15) wt.%, mo= (5-6) wt.%, zr= (5-6) wt.%, balance Ti.
2. Ingot casting preparation: nb is added in a NbTi intermediate alloy form, mo is added in a TiMo intermediate alloy form, zr is added in a zirconium sponge form, the rest is titanium sponge, the raw materials are weighed according to a proportion and mixed uniformly to prepare an electrode, and vacuum consumable smelting is adopted for three times to obtain an alloy ingot with the diameter phi 600mm, and the single weight of the ingot is about 3000kg.
3. Preparing a bar blank: forging and rolling the cast ingot to obtain a rolled rod with the diameter phi of 55mm, and peeling the surface of the rolled rod to obtain a heat treatment blank.
4. And (3) heat treatment: (1) solid solution: heating the blank to 820 ℃, preserving heat for 90 minutes, quickly putting the blank into flowing water to cool the blank to a room temperature state after the blank is heated to the temperature, and quickly transferring the blank into liquid nitrogen to carry out cryogenic treatment. (2) cyclic aging: the blank after liquid nitrogen treatment is heated to 520 ℃ again, kept for 2 hours, cooled to room temperature in air, heated to 460 ℃ again, kept for 2 hours, cooled to room temperature in air, subjected to heat treatment of the steps, and circulated for many times.
5. And (3) carrying out finishing machining on the bar blank after heat treatment to obtain the phi 50mm titanium alloy bar.
Example 3
Based on the above examples 1 and 2, the present example is specifically described by taking the production of Ti14.1Nb5.6Mo5.2Zr titanium alloy rods:
1. alloy design: the chemical components of the titanium alloy are as follows: nb=14.1 wt.%, mo=5.6 wt.%, zr=5.2 wt.%, balance Ti.
2. Ingot casting preparation: nb is added in a NbTi intermediate alloy form, mo is added in a TiMo intermediate alloy form, zr is added in a zirconium sponge form, the rest is titanium sponge, the raw materials are weighed according to a proportion and mixed uniformly to prepare an electrode, and vacuum consumable smelting is adopted for three times to obtain an alloy ingot with the diameter phi 600mm, and the single weight of the ingot is about 3000kg.
3. Preparing a bar blank: forging and rolling the cast ingot to obtain a rolled rod with the diameter phi of 55mm, and peeling the surface of the rolled rod to obtain a heat treatment blank.
4. Referring to fig. 1, fig. 1 shows a schematic process diagram of heat treatment in the present application, specifically including: (1) solid solution: heating the blank to 820 ℃, preserving heat for 90 minutes, quickly putting the blank into flowing water to cool the blank to a room temperature state after the blank is heated to the temperature, and quickly transferring the blank into liquid nitrogen to carry out cryogenic treatment. (2) cyclic aging: the blank after liquid nitrogen treatment is heated to 520 ℃ again, kept for 2 hours, cooled to room temperature in air, heated to 460 ℃ again, kept for 2 hours, cooled to room temperature in air, subjected to heat treatment of the steps, and circulated for many times.
5. And (3) finishing the bar blank after heat treatment to obtain a titanium alloy bar with the diameter of phi 50mm and the composition of Ti14.1Nb5.6Mo5.2Zr.
Example 4
Based on the foregoing example 1-example 3, this example gives a comparison of the overall properties of titanium alloy bars having a diameter of Φ50mm, specifically, 4A titanium alloy having a diameter of Φ50mm, ti6Al4V titanium alloy having a diameter of Φ50mm, ti14.1Nb5.6Mo5.2Zr titanium alloy bars having a diameter of Φ50mm prepared in this application were selected for comparison, and the results are shown in Table 1 below:
TABLE 1
As shown in Table 1, the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod with the diameter of phi 50mm provided by the application has the advantages that the tensile strength, the yield strength, the fatigue limit and the elastic modulus are all increased compared with those of the titanium alloy rod subjected to the solid solution and the secondary cycle aging treatment.
Comparing Ti14.1Nb5.6Mo5.2Zr titanium alloy rod with diameter phi 50mm with 4A titanium alloy with diameter phi 50 mm: whether the titanium alloy rod is subjected to primary cycle aging treatment or secondary cycle aging treatment, the tensile strength, the yield strength and the fatigue limit of the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod provided by the scheme are far superior to those of 4A titanium alloy with the diameter of phi 50mm, and in addition, the elastic modulus of the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod provided by the scheme is far lower than that of 4A titanium alloy with the diameter of phi 50 mm.
Comparing Ti14.1Nb5.6Mo5.2Zr titanium alloy rod with diameter phi 50mm with Ti6Al4V titanium alloy with diameter phi 50 mm: the tensile strength, the yield strength and the fatigue limit of the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod provided by the scheme are all superior to those of Ti6Al4V titanium alloy with the diameter of phi 50mm, and in addition, the elastic modulus of the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod provided by the scheme is far lower than that of Ti6Al4V titanium alloy with the diameter of phi 50 mm.
The comprehensive performance comparison of titanium alloy bars with the diameter of phi 60mm is given in the example, and specifically, 4A titanium alloy with the diameter of phi 60mm, ti6Al4V titanium alloy with the diameter of phi 60mm and Ti14.1Nb5.6Mo5.2Zr titanium alloy bars with the diameter of phi 60mm prepared by the method are selected for comparison.
TABLE 2
As shown in Table 2, the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod with the diameter of phi 60mm provided by the application has the advantages that the tensile strength, the yield strength, the fatigue limit and the elastic modulus are all increased compared with those of the titanium alloy rod subjected to the solid solution and the secondary cycle aging treatment.
Comparing Ti14.1Nb5.6Mo5.2Zr titanium alloy rod with diameter phi 60mm with 4A titanium alloy with diameter phi 60 mm: whether the titanium alloy rod is subjected to primary cycle aging treatment or secondary cycle aging treatment, the tensile strength, the yield strength and the fatigue limit of the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod provided by the scheme are far superior to those of 4A titanium alloy with the diameter of phi 60mm, and in addition, the elastic modulus of the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod provided by the scheme is far lower than that of 4A titanium alloy with the diameter of phi 60 mm.
Comparing Ti14.1Nb5.6Mo5.2Zr titanium alloy rod with diameter phi 60mm with Ti6Al4V titanium alloy with diameter phi 60 mm: the tensile strength, the yield strength and the fatigue limit of the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod provided by the scheme are all superior to those of Ti6Al4V titanium alloy with the diameter of phi 60mm, and in addition, the elastic modulus of the Ti14.1Nb5.6Mo5.2Zr titanium alloy rod provided by the scheme is far lower than that of Ti6Al4V titanium alloy with the diameter of phi 60 mm.
In summary, by adopting the high-performance titanium alloy for the artificial joint and the preparation method thereof, the titanium alloy material with high strength, low elastic modulus and excellent biocompatibility can be prepared, so that the use safety of the joint can be obviously improved, and the service life of the joint can be prolonged.
Other embodiments of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. This application is intended to cover any adaptations, uses, or adaptations of the disclosure following, in general, the principles of the disclosure and including such departures from the present disclosure as come within known or customary practice within the art to which the disclosure pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.
It is to be understood that the present disclosure is not limited to the precise arrangements and instrumentalities shown in the drawings, and that various modifications and changes may be effected without departing from the scope thereof. The scope of the present disclosure is limited only by the appended claims.
Claims (10)
1. The high-performance titanium alloy for the artificial joint is characterized by comprising the following chemical components in percentage by mass:
nb with the mass ratio of: (13-15 wt.%;
mo, the mass ratio is: (5-6 wt.%;
zr, the mass ratio is: (5-6 wt.%;
the balance being Ti.
2. The preparation method of the high-performance titanium alloy for the artificial joint is characterized by comprising the following steps of:
according to the component proportion of claim 1, raw materials are obtained and mixed uniformly;
smelting the uniformly mixed raw materials in a vacuum consumable manner to prepare alloy ingots;
forging and rolling the alloy cast ingot to obtain a rolled rod;
peeling the surface of the rolled rod to obtain a blank;
heat treating the blank to obtain a titanium alloy bar blank;
and (3) finishing the titanium alloy rod blank to obtain a titanium alloy rod, namely the high-performance titanium alloy for the artificial joint.
3. The method of producing a high-performance titanium alloy for artificial joints according to claim 2, wherein the step of heat-treating the ingot to obtain a titanium alloy rod blank comprises:
carrying out solid solution treatment on the blank;
and heating, preserving heat and cooling the blank subjected to the solution treatment, and circulating for a plurality of times to obtain a titanium alloy bar blank.
4. The method for producing a high-performance titanium alloy for artificial joints according to claim 3, wherein the step of subjecting the ingot to solution treatment comprises:
heating the blank to 820 ℃, and preserving heat for 90 minutes;
cooling the blank after heat preservation in flowing water to a room temperature state;
transferring the blank cooled to the room temperature state into liquid nitrogen for cryogenic treatment to obtain the blank after solution treatment.
5. The method for producing a high-performance titanium alloy for an artificial joint according to claim 3, wherein the step of heating-maintaining-cooling the solid solution-treated billet and circulating the same a plurality of times to obtain a titanium alloy rod billet comprises:
heating for the first time, heating the blank subjected to solution treatment to 520 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way;
heating for the second time, heating the blank subjected to the first heating treatment to 460 ℃, preserving heat for 2 hours, and cooling to room temperature in an air cooling way; obtaining the titanium alloy rod blank.
6. The method for producing a high-performance titanium alloy for an artificial joint according to claim 5, wherein the first heating and the second heating are performed at least once in this order to obtain the titanium alloy rod blank.
7. The method for producing a high-performance titanium alloy for artificial joints according to claim 2, wherein the steps of obtaining raw materials and mixing are as follows:
nb is added in the form of NbTi intermediate alloy, mo is added in the form of TiMo intermediate alloy, zr is added in the form of sponge zirconium, and the balance is sponge titanium.
8. The method for preparing high-performance titanium alloy for artificial joint according to claim 2, wherein the step of vacuum consumable melting the uniformly mixed raw materials to prepare an alloy ingot comprises:
preparing the uniformly mixed raw materials into an electrode;
carrying out vacuum consumable smelting on the electrode to obtain an alloy cast ingot;
wherein the alloy ingot has a diameter phi of 600mm and a single weight of about 3000kg.
9. The method for producing a high-performance titanium alloy for artificial joints according to claim 2, wherein the steps of forging and rolling the alloy ingot are performed to obtain a rolled rod, the diameter Φ55-95mm.
10. The method for producing a high-performance titanium alloy for artificial joints according to claim 2, wherein the diameter of the titanium alloy rod is Φ50-90mm.
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| CN116791016A (en) * | 2023-07-06 | 2023-09-22 | 哈尔滨工业大学 | Method for eliminating titanium-rich segregation of as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment |
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| CN116791016A (en) * | 2023-07-06 | 2023-09-22 | 哈尔滨工业大学 | Method for eliminating titanium-rich segregation of as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment |
| CN116791016B (en) * | 2023-07-06 | 2024-04-12 | 哈尔滨工业大学 | Method for eliminating titanium-rich segregation of as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment |
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