WO2019100809A1 - Titane pur à grain filamenteux à résistance et à ténacité élevées et son procédé de préparation - Google Patents

Titane pur à grain filamenteux à résistance et à ténacité élevées et son procédé de préparation Download PDF

Info

Publication number
WO2019100809A1
WO2019100809A1 PCT/CN2018/104167 CN2018104167W WO2019100809A1 WO 2019100809 A1 WO2019100809 A1 WO 2019100809A1 CN 2018104167 W CN2018104167 W CN 2018104167W WO 2019100809 A1 WO2019100809 A1 WO 2019100809A1
Authority
WO
WIPO (PCT)
Prior art keywords
filamentous
grains
titanium
pure titanium
annealing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2018/104167
Other languages
English (en)
Chinese (zh)
Inventor
黄崇湘
王艳飞
聂宇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sichuan University
Original Assignee
Sichuan University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sichuan University filed Critical Sichuan University
Priority to JP2020528249A priority Critical patent/JP6943513B2/ja
Publication of WO2019100809A1 publication Critical patent/WO2019100809A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Images

Classifications

    • 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
    • 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
    • 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
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • 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 invention belongs to the field of biosurgical implantable structural materials, and particularly relates to a filamentous crystal pure titanium material with high toughness and energy and a preparation method thereof.
  • pure titanium not only has a better biological phase. Capacitive and corrosion-resistant, it also avoids the expensive cost of the alloy, complex processes and elements such as Al and V which are harmful to living organisms. It can be preferably used as a structural material for joints, dental and scaffold organisms. However, conventional pure titanium exhibits lower yield strength and wear resistance due to the lack of strengthening of alloying elements.
  • the standard GB/T 13810-2007 (ISO 5832-2 2012) specifies the yield strengths of TA1 (Grade 1) and TA2 (Grade 2) pure titanium of 170 MPa and 275 MPa, respectively, which is much lower than the 860 MPa of Ti-6Al-4V. . Therefore, the development of pure titanium with ultra-high strength and toughness is an urgent problem to be solved as a load-bearing structural material.
  • the ultrafine or nanocrystalline structure formed by severe plastic deformation can effectively improve the strength of the metal material, the lattice defects such as saturated dislocations and grain boundaries severely limit the subsequent plastic deformation ability, so that after the type of material yields Immediately breaks the failure.
  • the use of large plastic deformation method at room temperature to refine the hexagonal structure of pure titanium has the problem of difficult deformation and easy cracking.
  • the patent CN 103981472 B achieves grain refinement by equal channel angular extrusion in the form of copper wrapping, the process requires copper wrapping, multi-pass equal channel corner extrusion, and removal of the wrapped copper, which is extremely inefficient. It is not suitable for large-scale production.
  • patent CN 102703756 B combined with high energy ball milling and spark plasma sintering process to prepare coarse-grain/fine-grain bimodal grain Ti-6Al-4V with better mechanical properties.
  • this process step is complicated and the energy consumption is high.
  • the limited toughness of the multimodal grain structure makes it difficult to make the strength of the pure titanium reach the strength of the alloy material.
  • the pure titanium with superior toughness can be prepared by asynchronous rolling and subsequent annealing, but the tensile strength of the whole material is still lower than 700 MPa, and the block size is only 300 ⁇ m, which is difficult to be practical.
  • the effect of ultrasonic impact treatment on the deformation behavior of the present pure titanium under uniaxial tension Materials and design, 2017; 117: 371–381., based on the mechanism of fine-grain strengthening and gradient structure coupling toughening, use The high-energy shot peening method prepares a nano-gradient layer on the surface of pure titanium.
  • the thickness of the nano-gradient layer is too thin, the yield strength is only increased by 60 MPa and the plasticity is greatly reduced.
  • the overall strength of the materials prepared by the surface mechanical nanometering method is not much improved, and the surface roughness is too large, which is not conducive to production and practical.
  • the pure titanium has the same tough mechanical properties as the alloy titanium, and has better biocompatibility and corrosion resistance, avoiding the expensive cost of the alloy, the complicated process and the elements such as Al and V which are harmful to the living body. It is preferably used as a structural material for implants, dental and scaffold organisms.
  • the invention also provides a preparation method of high-strength and tough filamentous crystal pure titanium.
  • a high-strength and tough filamentous grain pure titanium the microstructure consists of a mixture of filamentary grains and equiaxed grains, wherein the ratio of the major axis to the minor axis of the filamentous grains is greater than 40 and the minor axis size is 10 ⁇ m to 10 nm.
  • the equiaxed grains are recrystallized ultrafine grains.
  • the volume fraction of the filamentous crystal grains is more than 80%, and the difference in orientation between the long axes of the filamentary crystal grains is less than 10°.
  • the equiaxed grains are equiaxed ultrafine grains formed by partial recrystallization of a severely plastically deformed structure by short-time annealing.
  • the preparation method of the high-strength tough filamentous crystal pure titanium as described above comprises the following steps:
  • Step (1) The corner of the mold used for medium-channel corner extrusion is 120°.
  • step (2) the amount of strain for each rotary forging is ⁇ 1.4, and the cumulative strain for multi-pass swaging is ⁇ 2.5.
  • the annealing in the step (3) is a reductive annealing at a temperature of 300 to 400 ° C, and each annealing time is 60 s to 1 h.
  • the multi-pass control rolling process in the step (3) is synchronous symmetrical rolling along the longitudinal direction of the sheet, that is, the size and speed of the upper and lower rolls are the same and the rolling speed is not higher than 50 mm/s.
  • Step (3) The temperature range of the multi-pass control rolling process is -196 to 400 ° C, the strain of a single pass is ⁇ 0.1, and the cumulative strain of the multi-pass rolling between adjacent annealing is ⁇ 0.5.
  • the annealing process in the step (4) is a partial recrystallization annealing at a critical recrystallization temperature, the temperature is 400 to 450 ° C, and the time is 30 to 600 s.
  • the textured orientation of the filamentary grains of the filamentary crystal pure titanium produced along the long axis direction is a crystallographic soft orientation, and the equiaxed grains are discretely distributed between the filamentary grains.
  • the reason why the filamentary grain pure titanium has high strength and toughness is that: (1) ultrafine/nano-sized filamentary grains and equiaxed grains have high-density grain boundaries, which can effectively improve the yield strength of the material; (2) The recovered or recrystallized grains have lower dislocation density relative to the severely plastically deformed grains, providing more lattice defect storage space for subsequent work hardening; (3) discretely distributed between the filamentary grains Submicron and/or nano equiaxed crystals can effectively alleviate the stress concentration along the grain boundary caused by the uncoordinated deformation between filamentous grains, broaden the spatial range along the grain boundary strain gradient, and promote structural strengthening and toughening; (4) Compared with the equiaxed ultrafine or nanocrystalline, the dislocations have a sufficiently long sliding path along the long axis direction of the filamentary grains, and the soft orientation texture in this direction facilitates the actuation of the slip system, prompting the material to occur. Uniform plastic deformation.
  • the crystal grains are difficult to grow spontaneously in one direction;
  • the conventional severe plastic deformation method can change the shape of the parent metal grain, but the complex dislocation proliferation, quenching, and recombination process Grain refinement is evident and tends to form equiaxed dislocation structures or new grains.
  • the equal channel angular extrusion process has a circumferential confining pressure, but the large shear deformation at the corner causes the original grain to be broken and cannot be greatly elongated in one direction; the simple cumulative rolling process can be elongated.
  • the lamellar grain structure but the long diameter of these grains is relatively small; the drawing process does not have a large cumulative strain amount, and the aspect ratio of the formed crystal grains is also very small. Therefore, the preparation of the filamentary structure requires not only the accumulation of a sufficiently high plastic strain but also a suitable plastic deformation rate and path.
  • the purpose of a few passes of the equal channel corner extrusion step is to apply large strain to the bar and adjust the texture to reduce the angle between the grain slip system and the length direction of the rod, which is beneficial to the subsequent grain in the process of swaging.
  • the length direction is elongated and deformed.
  • the rotary forging process not only can apply uniform circumferential confining pressure, but the concentric unidirectional passage of variable diameter and the control single-pass strain are the key factors to ensure that the filamentary grains do not undergo equiaxed fracture.
  • the pure titanium after multi-pass swaging is recycled and annealed. And control rolling.
  • the filamentary grain pure titanium prepared by the method has the mechanical characteristics of having excellent strength and plastic deformation ability, the tensile yield strength is greater than 770 MPa, the tensile strength is greater than 900 MPa, and the uniform tensile plasticity is greater than 5%. The elongation after break is greater than 10%.
  • the present invention has the following advantages and beneficial effects:
  • microstructure composed of micro/nanofilamentous grains and ultrafine equiaxed grains can simultaneously exhibit various strengthening and toughening mechanisms of fine grain strengthening, non-uniform structure coupling strengthening and toughening, and texture toughening.
  • the pure titanium of the structure exhibits mechanical properties comparable to those of the alloy titanium;
  • the material prepared is practical, and the filamentary grain pure titanium overcomes the bottleneck of toughness and can replace the application of alloy titanium, especially for biosurgical implantable structural materials;
  • Fig. 1 is a graph showing the comparison of engineering stress-strain curves of the starting material, the pre-recrystallization pre-annealing material, and the filament-like grain materials obtained by different portions of recrystallization annealing conditions in Examples 1-3.
  • Figure 2 is a transmission electron micrograph (TEM) image of a cross section of a bar obtained after completion of multi-pass swaging in this Example 1.
  • TEM transmission electron micrograph
  • Example 3 is a three-dimensional metallographic diagram of the high-strength and tough filamentous crystal pure titanium prepared in Example 1, and it can be seen that the material is composed of ultrafine filamentary crystal grains.
  • Example 4 is an electron backscatter diffraction (EBSD) gray scale image of a 500 ⁇ 100 ⁇ m 2 region of high-strength tough filamentous crystal grains prepared in Example 1.
  • EBSD electron backscatter diffraction
  • Example 5 is an EBSD grayscale image of a 40 ⁇ 35 ⁇ m 2 region of high-strength and tough filamentous crystal grains prepared in Example 1, and black arrows indicate recrystallization superfine crystals.
  • Fig. 6 is a graph showing the comparison of the engineering stress-strain curves of the filament-like crystal pure titanium prepared in Example 4 (broken line) and Example 1 (solid line).
  • Fig. 7 is a EBSD gray scale diagram of a portion of a high-strength tough filamentous grain pure titanium partial 40 ⁇ 35 ⁇ m 2 prepared in Example 4.
  • Figure 8 is a graph showing the comparison of the engineering stress-strain curves of the filament-like crystal pure titanium prepared in Example 5 (broken line) and Example 1 (solid line).
  • the raw material grade is TA2, the technical standard is in accordance with GB/T3620.1-2007, and the composition is shown in Table 1.
  • the raw material is made into a standard tensile pattern.
  • the engineering stress-strain curve obtained by quasi-static tensile test is shown by the dotted line in Figure 1.
  • the yield strength is 280 MPa
  • the tensile strength is 430 MPa
  • the uniform elongation is 11.9%
  • the elongation after fracture It is 27%.
  • Raw material pure titanium rod with a diameter of 32 mm.
  • Two-pass equal channel angular extrusion The die with a channel diameter of 32 mm is selected, and the initial bar is subjected to the first pass equal channel angular extrusion.
  • the extrusion die has a rotation angle of 120° and an extrusion temperature of 400 ° C.
  • the bar is rotated 180° around the axis and placed in a mold for a second pass equal channel corner extrusion.
  • the first pass swaging is to forge the 32mm diameter bar obtained in step (1) to a diameter of 24mm, the strain is about 0.58; the second pass swaging will swallow the diameter of 24mm bar To a diameter of 16 mm, the strain should be about 0.81; the third pass swallowing will forge a diameter of 16 mm bar to a diameter of 8 mm, and the strain should be about 1.39.
  • the titanium rod having a diameter of 8 mm obtained in the step (2) was cut into a sheet having a cross section of 6.9 ⁇ 4 mm 2 , and the longitudinal direction of the sheet was parallel to the longitudinal direction of the swaged bar.
  • the sheet obtained in the step (3) was subjected to annealing in a vacuum furnace at a temperature of 350 ° C for a period of 600 s.
  • Multi-pass room temperature synchronous rolling the height of the roll is lowered by 0.1 mm, and the plate is rolled twice; the plate is fed in the direction of feeding, and the plate is further rolled twice.
  • Step (6) is repeated four more times, wherein the rolling direction is the length direction of the sheet and the strain of a single pass is less than 0.1.
  • the pure titanium obtained in the step (7) is subjected to annealing in a vacuum furnace at a temperature of 350 ° C for 600 s.
  • the pure titanium plate obtained in the foregoing step was subjected to partial recrystallization annealing in a vacuum furnace at a temperature of 450 ° C for 300 s.
  • the rolling process is room temperature rolling, in which the single pass rolling strain does not exceed 0.1, the cumulative plastic strain between adjacent annealings does not exceed 0.35, and the total cumulative plastic strain is 0.75.
  • Fig. 2 is a TEM microstructure of a cross section of a bar obtained after the multi-pass swaging of the step (2) in the present embodiment, and the grain profile is ultra-finely equiaxed.
  • Fig. 3 is a three-dimensional metallographic diagram of the high-strength and ductile grain-like pure titanium prepared in the present embodiment, and it can be seen that the material is composed of ultrafine filamentary grains.
  • Figure 4 is a EBSD grayscale image of a partial 500 x 100 m2 region of a pure titanium material prepared in this case. It can be seen that the body of the microstructure consists of elongated filamentary grains. The statistical results in this region show that the average length of the filamentous crystal grains is 166 ⁇ m, the average aspect ratio is 45.7, and the composition ratio of the filamentous crystal grains is 94%, and the orientation difference between the long axes of the filamentous crystal grains is smaller than 10°. Among them, the individual filamentous crystal grains have a length of 500 ⁇ m and an aspect ratio of more than 100.
  • Figure 5 is a EBSD grayscale image of a partial 40 x 35 ⁇ m 2 region of pure titanium material prepared in this case. Black arrows indicate that the recrystallized ultrafine crystals are discretely distributed along the filamentary grains.
  • the thin solid line in Fig. 1 is the quasi-static tensile test engineering stress-strain curve of the filamentous grain pure titanium in the rolling direction after the completion of step (9) in the case, and the yield strength and tensile strength are 973.7 MPa and 1030.3, respectively. MPa, but the uniform elongation is only 2.1%, and the elongation after fracture is greater than 7%
  • the thick solid line in Fig. 1 is the quasi-static tensile test engineering stress-strain curve of the filamentous grain pure titanium prepared in the step (10) of the present case, the yield strength is 770.5 MPa, and the tensile strength is 909.7 MPa.
  • the uniform elongation was 8.3%, and the elongation after break was greater than 15%.
  • This example differs from Example 1 in that the partial recrystallization annealing temperature of the preparation step (10) is 400 ° C for 480 s.
  • the thin dotted line in Figure 1 is the quasi-static tensile test engineering stress-strain curve of the filamentous grain pure titanium prepared in this case along the rolling direction.
  • the yield strength is as high as 838.2 MPa, with a very large work hardening rate and tensile strength. 964.8MPa, uniform plastic strain is 6.2%, elongation after fracture is greater than 12%.
  • the microstructure was similar to that of Example 1, but the degree of recovery and recrystallization ratio were reduced, and the composition ratio of filamentous crystal grains was about 99%.
  • This example differs from Example 1 in that the partial recrystallization annealing temperature of the preparation step (10) is 475 ° C for 300 s.
  • the thick dashed line in Figure 1 is the quasi-static tensile test engineering stress-strain curve of the filamentous grain pure titanium prepared in this case along the rolling direction.
  • the yield strength of the filamentous structure prepared in this case was reduced by about 90 MPa, while the uniform plasticity was only increased by 1.7%, and the elongation after fracture was greater than 16%.
  • the ratio of filamentous grain composition in the microstructure is reduced to 73%, which indicates that the filamentous grains have an important contribution to the toughness of the material.
  • the initial diameter of the raw material is 20 mm; the diameter of the channel of the extrusion die used in the step (1) is 20 mm; and the first pass of the step (2) is obtained by the step (1)
  • the 20mm diameter bar is swaged to a diameter of 16mm.
  • the second pass swaged swages a 16mm diameter bar to a diameter of 8mm.
  • the total cumulative plastic strain is only 1.833.
  • the subsequent steps are identical to those of Embodiment 1.
  • Fig. 6 is a comparison diagram of the engineering stress-strain curves of the filament-like structural material obtained before and after partial recrystallization in Example 1 and Example 1.
  • the yield strength and tensile strength of the filamentary grain material obtained before partial recrystallization annealing in this example were 740.8 MPa and 850.3 MPa, respectively.
  • the uniform elongation increased to 10.8%, and the elongation after fracture was greater than 20%, but the yield strength and tensile strength were 587.2 MPa and 707.2 MPa, respectively, which were much lower than those obtained in Example 1 and Example 2.
  • Figure 7 is a EBSD grayscale image of a partial 40 x 35 ⁇ m 2 region of a pure titanium material prepared in this case.
  • a small amount of recrystallized ultrafine crystals have a discrete distribution, and most of the crystal grains are filamentous.
  • the average minor axis size of the filamentary grains is much larger than that obtained in Example 1 and the distribution is extremely uneven, ranging from submicron spans to tens of micrometers.
  • Comparing the present embodiment with the first embodiment can show that the step (2) accumulating a sufficiently high plastic strain during the swaging process is favorable for forming uniform, fine filamentous crystal grains, and the size of the filamentous crystal grains seriously affects the material strength. Toughness properties, the smaller the diameter of the filamentary grains, the higher the material strength.
  • the temperature of the controlled rolling process is the liquid nitrogen temperature, that is, -196 ° C; in order to avoid the formation of cracks during the severe plastic deformation process at low temperature, the step (6) to the step of the rolling process ( 8) Performed a total of 4 times with a total cumulative plastic strain of 50% and a final sheet thickness of 2 mm.
  • the other steps and parameters are identical to those of the first embodiment.
  • Fig. 8 is a comparison diagram of the engineering stress-strain curves of the filament-like structural material obtained before and after partial recrystallization in Example (dashed line) and Example 1 (solid line).
  • the yield strength of the filamentous structural material obtained before partial recrystallization annealing in this example was 981.7 MPa, which was comparable to that obtained in the room temperature rolling of Example 1, but showed significant work hardening and tensile strength of 1072.3 MPa in the subsequent deformation process, and uniformity.
  • the elongation reached 3.4% and the elongation after break was greater than 7%.
  • the wire-like structural material obtained by vacuum annealing at 450 ° C for 300 s has a yield strength of 808.6 MPa, a tensile strength of 939.9 MPa, a uniform elongation of 7.4%, and an elongation after fracture of more than 14%.
  • the low temperature and large cumulative plastic deformation induced twinning is the reason why the strength of the filamentous structural material obtained in the present embodiment is higher than that obtained in Example 1.
  • the yield strength, tensile strength, and elongation after elongation of the filamentary grain pure titanium prepared in the above examples are in accordance with the Chinese National Standard (GB), the International Standardization Organization (ISO), and the American Society for Testing and Materials (ASTM).
  • the mechanical properties of pure titanium and titanium alloys for implantation were compared. The results are shown in Table 2.
  • the status bar in the table indicates the material supply status, including annealed state (A), cast state (W), cold worked state (CW), cold worked and partially recrystallized annealed state (CW+PRA); the table specifies the non-proportional extension strength (R p0.2 ) refers to the strength corresponding to 0.2% plastic strain, that is, the yield strength described in this patent.
  • the toughness of the filamentous crystal pure titanium provided by the present invention is much higher than that of the conventional surgical implanted pure titanium, and has the same properties as Ti-6Al-4V and Ti-6Al-7Nb. Quite mechanical properties.
  • the invention provides a high-strength and tough filamentous crystal pure titanium and a preparation method thereof, which are not limited to the application of biomedical surgical implantable structural materials. Any high-strength and tough filamentous crystal pure titanium provided by the invention and its preparation method in any field and industry are all covered by the patent.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Engineering & Computer Science (AREA)
  • Veterinary Medicine (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Dermatology (AREA)
  • Medicinal Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Forging (AREA)
  • Materials For Medical Uses (AREA)

Abstract

L'invention concerne un titane pur à grains filamenteux à résistance et à ténacité élevées, la microstructure étant formée de grains filamenteux ou de grains filamenteux mélangés à des grains équiaxes, le rapport de longueur de l'axe long à l'axe court des grains filamenteux étant supérieur à 40 et la taille de l'axe court étant de 10 µm à 10 nm, les grains équiaxes étant des grains ultrafins recristallisés. Le procédé de préparation comprend les étapes suivantes : (1) réalisation de 1 à 2 extrusions angulaires de canal égales en vue d'acquérir une barre de titane ; (2) réalisation d'un emboutissage de la barre de titane à multiples reprises, puis découpe en vue d'acquérir une plaque de titane présentant une section transversale rectangulaire ; (3) réalisation cyclique d'un recuit et laminage de commande de la plaque de titane à multiples reprises ; et (4) recuit en vue d'obtenir le titane pur à grains filamenteux à résistance et à ténacité élevées. Les propriétés mécaniques du titane pur obtenu sont équivalentes à l'alliage de titane, et les coûts sont réduits, ce qui permet d'éviter un traitement complexe et des éléments tels que Al et V qui sont nocifs pour des organismes vivants, étant donné qu'il est un matériau structural biologique implantable approprié pour les articulations, la dentisterie et les stents.
PCT/CN2018/104167 2017-11-22 2018-09-05 Titane pur à grain filamenteux à résistance et à ténacité élevées et son procédé de préparation Ceased WO2019100809A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2020528249A JP6943513B2 (ja) 2017-11-22 2018-09-05 高強靭性糸状結晶純チタンおよびその製造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201711173272.1 2017-11-22
CN201711173272.1A CN107881447B (zh) 2017-11-22 2017-11-22 一种高强韧性丝状晶粒纯钛及其制备方法

Publications (1)

Publication Number Publication Date
WO2019100809A1 true WO2019100809A1 (fr) 2019-05-31

Family

ID=61777961

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2018/104167 Ceased WO2019100809A1 (fr) 2017-11-22 2018-09-05 Titane pur à grain filamenteux à résistance et à ténacité élevées et son procédé de préparation

Country Status (3)

Country Link
JP (1) JP6943513B2 (fr)
CN (1) CN107881447B (fr)
WO (1) WO2019100809A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112160029A (zh) * 2020-09-27 2021-01-01 南京理工大学 一种准单晶管材及其制备方法
CN115415356A (zh) * 2022-08-29 2022-12-02 南京理工大学 一种具有网状纳米结构的异构铝合金棒材及其制备方法

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107881447B (zh) * 2017-11-22 2019-04-23 四川大学 一种高强韧性丝状晶粒纯钛及其制备方法
CN110063805B (zh) * 2019-05-13 2021-08-27 四川大学 一种纯钛牙种植体/微种植体及其制备方法
CN110195200B (zh) * 2019-06-13 2021-02-19 四川大学 一种纤维晶增韧高强度超细晶纯钛及其制备方法
CN110129699B (zh) * 2019-06-13 2020-05-12 中国科学院力学研究所 一种高均匀伸长率GPa级钛及其制备方法
CN110732665B (zh) * 2019-10-25 2021-07-23 昆明理工大学 一种梯度钛材料的制备方法
CN112662971B (zh) * 2020-10-28 2022-05-20 西安交通大学 一种具有梯度结构的高强twip钛合金及其热轧方法
CN113181423B (zh) * 2021-05-26 2022-02-08 四川大学 表面原位生长纳米羟基磷灰石的钛材料及制备方法和应用
JP7464330B2 (ja) * 2021-06-07 2024-04-09 株式会社丸ヱム製作所 スクリュー用母材、スクリューとその製造方法
CN114214584B (zh) * 2021-11-16 2022-08-23 四川大学 一种低温1800MPa级超高强度纯钛及其应用
CN114150243B (zh) * 2021-11-26 2022-08-19 中国航发北京航空材料研究院 一种超细等轴组织tc4钛合金丝材制备方法
CN115261670B (zh) * 2022-07-08 2023-07-07 四川大学 一种高强韧纯钛及其制备方法
CN115717225B (zh) * 2022-11-24 2023-10-17 河南科技大学 一种细化钛材晶粒的复合形变热处理工艺
KR20250120409A (ko) 2022-12-14 2025-08-08 가부시키가이샤 마루에무 세이사쿠쇼 스크루용 모재, 스크루와 그의 제조 방법
CN122038955B (zh) * 2026-04-16 2026-08-07 湘潭大学 一种具有优异抗断裂性能的强、弱多尺度界面共增韧纯钛及其制备方法
CN122099758A (zh) * 2026-04-24 2026-05-29 湘潭大学 一种具有表面拓扑结构的纯钛及其制备方法

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005074457A2 (fr) * 2003-12-15 2005-08-18 The Regents Of The University Of California Procede de preparation d'une feuille metallique a grains ultrafins
CN1745922A (zh) * 2005-09-15 2006-03-15 上海交通大学 微/纳米晶工业纯钛块材等径弯角挤压制备方法
US20060213592A1 (en) * 2004-06-29 2006-09-28 Postech Foundation Nanocrystalline titanium alloy, and method and apparatus for manufacturing the same
CN101219444A (zh) * 2008-01-14 2008-07-16 西安建筑科技大学 高强度工业纯钛块材室温等径弯曲通道变形制备方法
CN101624690A (zh) * 2009-08-10 2010-01-13 西安建筑科技大学 难变形金属块材室温等径弯曲通道变形制备方法
JP4686700B2 (ja) * 2003-10-01 2011-05-25 独立行政法人産業技術総合研究所 微細組織チタン及びその製造方法
CN103981472A (zh) * 2014-05-06 2014-08-13 西北工业大学 一种等径通道挤压制备超细晶纯钛的方法
CN107881447A (zh) * 2017-11-22 2018-04-06 四川大学 一种高强韧性丝状晶粒纯钛及其制备方法

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4000270C2 (de) * 1990-01-08 1999-02-04 Stahlwerk Ergste Gmbh & Co Kg Verfahren zum Kaltverformen von unlegiertem Titan
JPH07124242A (ja) * 1993-11-09 1995-05-16 Nikon Corp インプラント
JPH0853726A (ja) * 1994-08-09 1996-02-27 Nippon Steel Corp ロール成形用純チタン薄板およびその製造方法
JP5166921B2 (ja) * 2008-03-10 2013-03-21 株式会社神戸製鋼所 高強度で成形性に優れたチタン合金板
RU2383654C1 (ru) * 2008-10-22 2010-03-10 Государственное образовательное учреждение высшего профессионального образования "Уфимский государственный авиационный технический университет" Наноструктурный технически чистый титан для биомедицины и способ получения прутка из него
JP2016000848A (ja) * 2014-06-11 2016-01-07 株式会社神戸製鋼所 チタン合金鍛造材
JP2016023315A (ja) * 2014-07-16 2016-02-08 株式会社神戸製鋼所 チタン板およびその製造方法
CN105772503A (zh) * 2015-12-27 2016-07-20 佛山市领卓科技有限公司 高强度纯钛的制备方法
JP6737686B2 (ja) * 2016-10-24 2020-08-12 国立大学法人豊橋技術科学大学 純チタン金属ワイヤおよびその加工方法
CN106636747B (zh) * 2016-12-29 2018-06-05 广东技术师范学院 一种采用中厚板轧机二次退火生产工业纯钛板的制造方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4686700B2 (ja) * 2003-10-01 2011-05-25 独立行政法人産業技術総合研究所 微細組織チタン及びその製造方法
WO2005074457A2 (fr) * 2003-12-15 2005-08-18 The Regents Of The University Of California Procede de preparation d'une feuille metallique a grains ultrafins
US20060213592A1 (en) * 2004-06-29 2006-09-28 Postech Foundation Nanocrystalline titanium alloy, and method and apparatus for manufacturing the same
CN1745922A (zh) * 2005-09-15 2006-03-15 上海交通大学 微/纳米晶工业纯钛块材等径弯角挤压制备方法
CN101219444A (zh) * 2008-01-14 2008-07-16 西安建筑科技大学 高强度工业纯钛块材室温等径弯曲通道变形制备方法
CN101624690A (zh) * 2009-08-10 2010-01-13 西安建筑科技大学 难变形金属块材室温等径弯曲通道变形制备方法
CN103981472A (zh) * 2014-05-06 2014-08-13 西北工业大学 一种等径通道挤压制备超细晶纯钛的方法
CN107881447A (zh) * 2017-11-22 2018-04-06 四川大学 一种高强韧性丝状晶粒纯钛及其制备方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112160029A (zh) * 2020-09-27 2021-01-01 南京理工大学 一种准单晶管材及其制备方法
CN112160029B (zh) * 2020-09-27 2022-06-21 南京理工大学 一种准单晶管材及其制备方法
CN115415356A (zh) * 2022-08-29 2022-12-02 南京理工大学 一种具有网状纳米结构的异构铝合金棒材及其制备方法

Also Published As

Publication number Publication date
CN107881447A (zh) 2018-04-06
CN107881447B (zh) 2019-04-23
JP2021508764A (ja) 2021-03-11
JP6943513B2 (ja) 2021-10-06

Similar Documents

Publication Publication Date Title
CN107881447B (zh) 一种高强韧性丝状晶粒纯钛及其制备方法
US11891679B2 (en) High-strength and low-modulus β-type Si-containing titanium alloy, preparation method therefor and use thereof
Yu et al. High strength and toughness of Ti–6Al–4V sheets via cryorolling and short-period annealing
EP2868759B1 (fr) ALLIAGE DE Ti DU TYPE ALPHA + BETA ET SON PROCESSUS DE PRODUCTION
Seipp et al. Microstructure, crystallographic texture and mechanical properties of the magnesium alloy AZ31B after different routes of thermo-mechanical processing
US9624565B2 (en) Nanocrystal-containing titanium alloy and production method therefor
CN110004367A (zh) 一种氧化物弥散强化FeCrAl合金管材的制备方法
Semenova et al. Mechanical behavior and impact toughness of the ultrafine-grained Grade 5 Ti alloy processed by ECAP
CN112522650A (zh) 一种高强高韧超细孪晶纯钛及其制备方法
CN107574394A (zh) 一种医用超细晶tc4钛合金板材的制备方法
CN116460235B (zh) 一种制备异构等轴组织钛合金锻件的高温-深冷复合锻造方法
Valiev et al. Bulk nanostructured materials by SPD processing: techniques, microstructures and properties
CN119464988A (zh) 一种同时提高工业纯钛强度和延展性的方法
Zhang et al. Effect of forging steps on microstructure evolution and mechanical properties of Ti-6Al-4V alloy during multidirectional isothermal forging
CN110802125B (zh) 一种镁合金棒材的制备方法
Gao et al. Comparative investigation of deformation mechanisms in Ti-6Mo-3.5 Cr-1Zr metastable β titanium alloy subject to cold rolling strain paths
KR101414505B1 (ko) 고강도 및 고성형성을 가지는 티타늄 합금의 제조방법 및 이에 의한 티타늄 합금
CN120888851A (zh) 一种基于双相竞争的β钛合金细晶锻坯制备方法
Mashekova et al. Ultrafinegrained structure of D16 aluminium alloy after rolling in the corrugated rolls and on the longitudinal-wedge mill
CN120587379A (zh) 一种超细晶Ti-Zr合金棒材及其制备方法和应用
JPWO2018030231A1 (ja) 純チタン金属材料薄板の製造方法およびスピーカ振動板の製造方法
CN110195200B (zh) 一种纤维晶增韧高强度超细晶纯钛及其制备方法
CN115612955B (zh) 一种再结晶型高强韧超细晶纯钛及其制备方法
CN115055532B (zh) 一种兼具高强度和高塑性的钴铬基合金无缝管制备方法
CN114214584B (zh) 一种低温1800MPa级超高强度纯钛及其应用

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 18881896

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2020528249

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 18881896

Country of ref document: EP

Kind code of ref document: A1