CN107574394A - A kind of preparation method of medical ultra-fine grain TC4 titanium alloy plates - Google Patents
A kind of preparation method of medical ultra-fine grain TC4 titanium alloy plates Download PDFInfo
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Abstract
The invention provides a kind of preparation method of medical ultra-fine grain TC4 titanium alloy plates, this method includes：First, multiway forging is carried out to a diameter of 90mm~410mm TC4 titanium alloys billet, the TC4 titanium alloy slabs that thickness is 25mm~130mm is obtained after cooling；2nd, TC4 titanium alloy slabs are subjected to reconditioning, annealing and warm-rolling successively, the TC4 titanium alloy plates that thickness is 6mm~26mm is obtained after air cooling；3rd, TC4 titanium alloy plates are made annealing treatment, Ultra-fine Grained TC4 titanium alloy plate semi-finished product is obtained after air cooling；4th, Ultra-fine Grained TC4 titanium alloy plates semi-finished product are sheared successively, reconditioning, leveling, polishing, polishing and pickling, obtain the Ultra-fine Grained TC4 titanium alloy plates that thickness is 5mm~25mm.Multiway forging technique and warm-rolling technique are combined by the present invention, and the crystallite dimension for obtaining medical ultra-fine grain TC4 titanium alloy plates is 0.1 μm~1 μm, and surfacing, even tissue, good mechanical properties, meet the regulation of the standards of GB/T13810 2007.
Description
Technical field
The invention belongs to titanium alloy material processing technique field, and in particular to a kind of medical ultra-fine grain TC4 titanium alloy plates
Preparation method.
Background technology
More than 80% titanium alloy raw material are TC4 titanium alloys in medicine equipment both at home and abroad at present, are mainly used in making mouth
The implantation instruments such as the gear division such as chamber corona, fixed bridge, denture class, joint type and wound class.Research finds, the property of metal material
Can be closely related with its crystallite dimension, when the crystallite dimension of metal is refine to below 1 μm, can obtain by uniform equiax crystal group
The super fine crystal material to be occupied the majority into, high-angle boundary, super fine crystal material have high intensity, have super modeling under high temperature at room temperature
Property.Ultra-fine Grained TC4 titanium alloys have higher intensity, more preferable fatigue behaviour and stronger compared with common TC4 titanium alloys
Decay resistance, had broad application prospects in field of medical materials.
Forced plasticity deforming method be international material educational circles generally acknowledge prepare the most promising method of bulk ultrafine-grained materials, can will
The crystal grain refinement of coarse grained metal is to nanometer scale, and the super fine crystal material of preparation is by with highdensity crystal boundary and relatively low atomic density
Intergranular district's groups into the typical sizes of its crystalline region or further feature length are (0.1 μm of sub-micron at least in one-dimensional square
~1 μm)/nanometer (＜ 100nm).
The forced plasticity deforming method of titanium alloy mainly includes：Equal channel angular pressing (ECAP), high pressure and torsion (HPT), tire out
Product ply rolling method (ARB) and multiway forging method (MF).Equal channel angle method and high pressure and torsion can be used to prepare three-dimensional dimension less
Ultra fine grained steel bar, it is the main method of industrialized production Ultra-fine Grained titanium, but yield is relatively low, and plasticity to titanium alloy material,
Equipment and mold requires high；Accumulation ply rolling method can produce the thin plate and foil material of relatively thin size, and accumulate the work of ply rolling method
Sequence is complicated, easily produces jacket waste material；Multiway forging method is brilliant to reach refinement by implementing deformation to titanium alloy from different directions
Grain, the purpose for improving material property, experimental exploration is carried out using the titanium alloy plate of reduced size (thickness is less than 90mm) mostly,
And the equipment and moulds of industrial equipment used costly with it is special, the Ultra-fine Grained sheet metal thickness prepared by multiway forging method is 2mm,
Long a width of 300mm × 200mm, is not easy to be processed, and rough surface, and flatness is poor, and mechanical property is bad, it is difficult to meets doctor
Learn and require.
The content of the invention
The technical problems to be solved by the invention are to be directed to above-mentioned the deficiencies in the prior art, there is provided a kind of medical ultra-fine grain
The preparation method of TC4 titanium alloy plates.This method, will be multidirectional using a diameter of 90mm~410mm TC4 titanium alloys billet as raw material
Forging technology and warm-rolling technique are combined, and the crystallite dimension of the medical ultra-fine grain TC4 titanium alloy plates of preparation is 0.1 μm~1 μm,
Thickness is 5mm~25mm, tensile strength be 1050MPa~1300MPa, it is specified that nonproportional cyclic straining be 1000MPa~
1080MPa, elongation after fracture are 14%~17%；This method technique is simple, it is easy to accomplish, the requirement to equipment is low, can meet
The industrial production demand of Ultra-fine Grained TC4 titanium alloys.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of medical ultra-fine grain TC4 titanium alloy plates
Preparation method, it is characterised in that this method comprises the following steps：
Step 1: multiway forging, cooling are carried out to a diameter of 90mm~410mm TC4 titanium alloys billet using quick forging machine
The TC4 titanium alloy slabs that thickness is 25mm~130mm are obtained afterwards；Along the three-dimensional side of TC4 titanium alloy billets in the multiway forging
One cycle is unidirectionally forged to three times to what is carried out successively, and each deflection unidirectionally forged is 40%~60%；It is described
Multiway forging includes 2~4 circulations；The initial forging temperature of 1st circulation is 1050 DEG C~1150 DEG C, and final forging temperature is not less than
700 DEG C, the initial forging temperature circulated described in the 2nd time~the 4th is 700 DEG C~1000 DEG C, and final forging temperature is not less than 600 DEG C；
Step 2: the TC4 titanium alloy slabs obtained in step 1 are first carried out into reconditioning, then made annealing treatment, Ran Hou
Multi-pass warm-rolling is carried out under conditions of 550 DEG C~700 DEG C, the TC4 titanium alloy plates that thickness is 6mm~26mm are obtained after air cooling；
The pass deformation of the warm-rolling is 10%~20%, and the total deformation of the warm-rolling is not less than 50%；
Step 3: the TC4 titanium alloy plates obtained in step 2 are made annealing treatment, Ultra-fine Grained TC4 is obtained after air cooling
Titanium alloy plate semi-finished product；
Step 4: the Ultra-fine Grained TC4 titanium alloy plates semi-finished product obtained in step 3 are sheared successively, reconditioning, rectify
Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plates that thickness is 5mm~25mm.
The preparation method of above-mentioned a kind of medical ultra-fine grain TC4 titanium alloy plates, it is characterised in that fast described in step 1
Forging machine is die hammer or hydraulic press.
The preparation method of above-mentioned a kind of medical ultra-fine grain TC4 titanium alloy plates, it is characterised in that moved back described in step 2
The temperature of fire processing is 550 DEG C~700 DEG C, and the time is 60min~80min.
The preparation method of above-mentioned a kind of medical ultra-fine grain TC4 titanium alloy plates, it is characterised in that moved back described in step 3
The temperature of fire processing is 500 DEG C~650 DEG C, and the time is 30min~60min.
The preparation method of above-mentioned a kind of medical ultra-fine grain TC4 titanium alloy plates, it is characterised in that rectified described in step 4
Flat temperature is 400 DEG C~500 DEG C.
The present invention has advantages below compared with prior art：
1st, it is combined using multiway forging technique and warm-rolling technique in the present invention, is refined first using multiway forging method
The crystallite dimension of TC4 titanium alloys and the growth for suppressing texture, anisotropy is avoided, reduce the deformation temperature of TC4 titanium alloys
Degree, and optimal rate of deformation is improved, then by warm-rolling, improve sheet material flatness under mesophilic condition, while continue to become
Shape makes the crystal grain of TC4 titanium alloys further refine, final to obtain the medical ultra-fine grain TC4 titaniums conjunction that crystallite dimension is 0.1 μm~1 μm
Golden plate material, the surfacing of medical ultra-fine grain TC4 titanium alloy plates, even tissue.
2nd, the present invention using a diameter of 90mm~410mm TC4 titanium alloys billet as raw material, be prepared thickness for 5mm~
25mm medical ultra-fine grain TC4 titanium alloy plates, the size range of raw material is expanded, improve the machinability of product, the doctor
Tensile strength with Ultra-fine Grained TC4 titanium alloy plates is 1050MPa~1300MPa, it is specified that nonproportional cyclic straining is 1000MPa
~1080MPa, elongation after fracture are 14%~17%, meet GB/T13810-2007 regulation, and be better than existing product.
3rd, technique of the invention is simple, it is easy to accomplish, the requirement to equipment is low, can be real in common quick forging machine and milling train
The preparation of existing medical ultra-fine grain TC4 titanium alloys, meet the industrial production demand of medical ultra-fine grain TC4 titanium alloys.
The present invention is described in further detail with reference to the accompanying drawings and examples.
Brief description of the drawings
Fig. 1 is the schematic diagram of multiway forging technical process of the present invention.
Fig. 2 is the TEM figures of medical ultra-fine grain TC4 titanium alloy plates prepared by the embodiment of the present invention 1.
Fig. 3 is the TEM figures of medical ultra-fine grain TC4 titanium alloy plates prepared by the embodiment of the present invention 3.
Embodiment
Fig. 1 is multiway forging technical process schematic diagram of the present invention, and filled black arrows direction represents what is unidirectionally forged in figure
Three directions (being respectively X-axis, Y-axis and the Z-direction of TC4 titanium alloy billets).As seen from Figure 1, the 1st time of multiway forging
In cyclic process, along the axis direction of TC4 titanium alloy billets, to be Y direction carried out to the end faces of TC4 titanium alloy billets the first
Once unidirectional forging, then forge piece is rotated by 90 ° along Z-direction and carries out second of unidirectional forging, is finally rotated by 90 ° again along X
Direction of principal axis carries out the unidirectional forging of third time, completes the 1st circulation；In 2nd time~4 times cyclic processes of multiway forging, first along Y
Direction of principal axis carries out unidirectional forging for the first time to forge piece, and then forge piece is rotated by 90 ° along Z-direction and carries out second of unidirectional forging
Make, be finally rotated by 90 ° again along X-direction and carry out the unidirectional forging of third time, complete single cycle, repeat single cycle, complete more
To the 2nd time~4 times circulations of forging.
Embodiment 1
The preparation method of the present embodiment comprises the following steps：
Step 1: carrying out multiway forging to a diameter of 410mm TC4 titanium alloys billet using hydraulic press, obtained after cooling
Thickness is 130mm TC4 titanium alloy slabs；Carried out successively along the three-dimensional of TC4 titanium alloy billets in the multiway forging
One cycle is unidirectionally forged to three times, and each deflection unidirectionally forged is 60%；The multiway forging includes 4 circulations,
The initial forging temperature of 1st circulation is 1150 DEG C, and final forging temperature is 715 DEG C, and the initial forging temperature of the 2nd circulation is 950
DEG C, 602 DEG C of final forging temperature, the initial forging temperature of the 3rd circulation is 800 DEG C, 610 DEG C of final forging temperature, is circulated described in the 4th
Initial forging temperature is 700 DEG C, 617 DEG C of final forging temperature；
Step 2: by after the TC4 titanium alloy slab reconditionings obtained in step 1, insulation 80min enters under conditions of 700 DEG C
Row annealing, then carries out three passage warm-rollings under conditions of 700 DEG C, and the TC4 titanium alloys that thickness is 26mm are obtained after air cooling
Sheet material；The pass deformation of the warm-rolling is 20%, and the total deformation of the warm-rolling is 60%；
Annealed Step 3: the TC4 titanium alloy plates obtained in step 2 are incubated into 60min under conditions of 650 DEG C
Handle, Ultra-fine Grained TC4 titanium alloy plate semi-finished product are obtained after air cooling；
Step 4: the Ultra-fine Grained TC4 titanium alloy plates semi-finished product obtained in step 3 are sheared successively, reconditioning, rectify
Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plates that thickness is 25mm；The temperature of the leveling is
500℃。
Fig. 2 is that the TEM of medical ultra-fine grain TC4 titanium alloy plates manufactured in the present embodiment schemes, as can be seen from Figure 2 embodiment
The interior tissue of the medical ultra-fine grain TC4 titanium alloy plates of preparation is uniform, and crystallite dimension is 0.5 μm~1 μm.
Embodiment 2
The preparation method of the present embodiment comprises the following steps：
Step 1: carrying out multiway forging to a diameter of 150mm TC4 titanium alloys billet using die hammer, obtained after cooling
Thickness is 130mm TC4 titanium alloy slabs；Carried out successively along the three-dimensional of TC4 titanium alloy billets in the multiway forging
One cycle is unidirectionally forged to three times, and each deflection unidirectionally forged is 45%；The multiway forging includes 2 circulations,
The initial forging temperature of 1st circulation is 1150 DEG C, and final forging temperature is 700 DEG C, and the initial forging temperature of the 2nd circulation is 900
DEG C, 634 DEG C of final forging temperature；
Step 2: by after the TC4 titanium alloy slab reconditionings obtained in step 1, insulation 60min enters under conditions of 630 DEG C
Row annealing, then carries out five passage warm-rollings under conditions of 630 DEG C, and the TC4 titanium alloys that thickness is 11mm are obtained after air cooling
Sheet material；The pass deformation of the warm-rolling is 10%, and the total deformation of the warm-rolling is 50%；
Annealed Step 3: the TC4 titanium alloy plates obtained in step 2 are incubated into 40min under conditions of 550 DEG C
Handle, Ultra-fine Grained TC4 titanium alloy plate semi-finished product are obtained after air cooling；
Step 4: the Ultra-fine Grained TC4 titanium alloy plates semi-finished product obtained in step 3 are sheared successively, reconditioning, rectify
Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plates that thickness is 10mm；The temperature of the leveling is
430℃。
After testing, the crystallite dimension of medical ultra-fine grain TC4 titanium alloy plates manufactured in the present embodiment is 0.8 μm~1 μm.
Embodiment 3
The preparation method of the present embodiment comprises the following steps：
Step 1: carrying out multiway forging to a diameter of 210mm TC4 titanium alloys billet using hydraulic press, obtained after cooling
Thickness is 65mm TC4 titanium alloy slabs；Three carried out successively along the three-dimensional of TC4 titanium alloy billets in the multiway forging
Secondary to be unidirectionally forged to one cycle, each deflection unidirectionally forged is 50%；The multiway forging includes 3 and circulated, and the 1st
The initial forging temperature of the secondary circulation is 1050 DEG C, and final forging temperature is 718 DEG C, and the initial forging temperature of the 2nd circulation is 950 DEG C,
615 DEG C of final forging temperature, the initial forging temperature of the 3rd circulation is 700 DEG C, 600 DEG C of final forging temperature；
Step 2: by after the TC4 titanium alloy slab reconditionings obtained in step 1, insulation 80min enters under conditions of 650 DEG C
Row annealing, then carries out three passage warm-rollings under conditions of 650 DEG C, and the TC4 titanium alloys that thickness is 26mm are obtained after air cooling
Sheet material；The pass deformation of the warm-rolling is 20%, and the total deformation of the warm-rolling is 60%；
Annealed Step 3: the TC4 titanium alloy plates obtained in step 2 are incubated into 60min under conditions of 600 DEG C
Handle, Ultra-fine Grained TC4 titanium alloy plate semi-finished product are obtained after air cooling；
Step 4: the Ultra-fine Grained TC4 titanium alloy plates semi-finished product obtained in step 3 are sheared successively, reconditioning, rectify
Flat, polishing, polishing and pickling, it is 15mm medical ultra-fine grain TC4 titanium alloy plates to obtain thickness；The temperature of the leveling is 450
℃。
Fig. 3 is that the TEM of medical ultra-fine grain TC4 titanium alloy plates manufactured in the present embodiment schemes, this implementation as can be seen from Figure 3
The interior tissue of medical ultra-fine grain TC4 titanium alloy plates prepared by example is uniform, and crystallite dimension is 0.4 μm~0.6 μm.
Embodiment 4
The preparation method of the present embodiment comprises the following steps：
Step 1: carrying out multiway forging to a diameter of 350mm TC4 titanium alloys billet using hydraulic press, obtained after cooling
Thickness is 100mm TC4 titanium alloy slabs；Carried out successively along the three-dimensional of TC4 titanium alloy billets in the multiway forging
One cycle is unidirectionally forged to three times, and each deflection unidirectionally forged is 55%；The multiway forging includes 4 circulations,
The initial forging temperature of 1st circulation is 1100 DEG C, and final forging temperature is 706 DEG C, and the initial forging temperature of the 2nd circulation is 900
DEG C, 612 DEG C of final forging temperature, the initial forging temperature of the 3rd circulation is 850 DEG C, 607 DEG C of final forging temperature, is circulated described in the 4th
Initial forging temperature is 800 DEG C, 619 DEG C of final forging temperature；
Step 2: by after the TC4 titanium alloy slab reconditionings obtained in step 1, insulation 70min enters under conditions of 650 DEG C
Row annealing, then carries out three passage warm-rollings under conditions of 650 DEG C, and the TC4 titanium alloys that thickness is 21mm are obtained after air cooling
Sheet material；The pass deformation of the warm-rolling is 20%, and the total deformation of the warm-rolling is 60%；
Annealed Step 3: the TC4 titanium alloy plates obtained in step 2 are incubated into 40min under conditions of 600 DEG C
Handle, Ultra-fine Grained TC4 titanium alloy plate semi-finished product are obtained after air cooling；
Step 4: the Ultra-fine Grained TC4 titanium alloy plates semi-finished product obtained in step 3 are sheared successively, reconditioning, rectify
Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plates that thickness is 20mm；The temperature of the leveling is
450℃。
After testing, the crystallite dimension of medical ultra-fine grain TC4 titanium alloy plates manufactured in the present embodiment is 0.6 μm~0.8 μm.
Embodiment 5
The preparation method of the present embodiment Ultra-fine Grained TC4 titanium alloy plates comprises the following steps：
Step 1: carrying out multiway forging to a diameter of 90mm TC4 titanium alloys billet using die hammer, thickness is obtained after cooling
Spend the TC4 titanium alloy slabs for 25mm；Carried out successively three times along the three-dimensional of TC4 titanium alloy billets in the multiway forging
One cycle unidirectionally is forged to, each deflection unidirectionally forged is 40%；The multiway forging includes 2 and circulated, the 1st time
The initial forging temperature of the circulation is 1050 DEG C, and final forging temperature is 719 DEG C, and the initial forging temperature of the 2nd circulation is 700 DEG C, eventually
Forge 600 DEG C of temperature；
Step 2: by after the TC4 titanium alloy slab reconditionings obtained in step 1, insulation 60min enters under conditions of 550 DEG C
Row annealing, four-pass warm-rolling is then carried out under conditions of 550 DEG C, the TC4 titanium alloy sheets that thickness is 6mm are obtained after air cooling
Material；The pass deformation of the warm-rolling is 15%, and the total deformation of the warm-rolling is 60%；
Annealed Step 3: the TC4 titanium alloy plates obtained in step 2 are incubated into 30min under conditions of 500 DEG C
Handle, Ultra-fine Grained TC4 titanium alloy plate semi-finished product are obtained after air cooling；
Step 4: the Ultra-fine Grained TC4 titanium alloy plates semi-finished product obtained in step 3 are sheared successively, reconditioning, rectify
Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plates that thickness is 5mm；The temperature of the leveling is 400
℃。
After testing, the crystallite dimension of medical ultra-fine grain TC4 titanium alloy plates manufactured in the present embodiment is 0.7 μm~0.9 μm.
Embodiment 6
The preparation method of the present embodiment comprises the following steps：
Step 1: carrying out multiway forging to a diameter of 115mm TC4 titanium alloys billet using die hammer, obtained after cooling
Thickness is 35mm TC4 titanium alloy slabs；Three carried out successively along the three-dimensional of TC4 titanium alloy billets in the multiway forging
Secondary to be unidirectionally forged to one cycle, each deflection unidirectionally forged is 44%；The multiway forging includes 4 and circulated, and the 1st
The initial forging temperature of the secondary circulation is 1050 DEG C, and final forging temperature is 706 DEG C, and the initial forging temperature of the 2nd circulation is 1000 DEG C,
613 DEG C of final forging temperature, the initial forging temperature of the 3rd circulation is 1000 DEG C, 602 DEG C of final forging temperature, the beginning circulated described in the 4th
It is 1000 DEG C to forge temperature, 607 DEG C of final forging temperature；
Step 2: by after the TC4 titanium alloy slab reconditionings obtained in step 1, insulation 60min enters under conditions of 600 DEG C
Row annealing, then carries out warm-rolling under conditions of 600 DEG C, and the TC4 titanium alloy plates that thickness is 7mm are obtained after air cooling；Institute
The pass deformation for stating warm-rolling is 16%, and the total deformation of the warm-rolling is 80%；
Annealed Step 3: the TC4 titanium alloy plates obtained in step 2 are incubated into 30min under conditions of 500 DEG C
Handle, Ultra-fine Grained TC4 titanium alloy plate semi-finished product are obtained after air cooling；
Step 4: the Ultra-fine Grained TC4 titanium alloy plates semi-finished product obtained in step 3 are sheared successively, reconditioning, rectify
Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plates that thickness is 5mm；The temperature of the leveling is 450
℃。
After testing, the crystallite dimension of medical ultra-fine grain TC4 titanium alloy plates manufactured in the present embodiment is 0.1 μm~0.5 μm.
Comparative example 1
The preparation method of this comparative example comprises the following steps：
Step 1: carrying out multiway forging to a diameter of 115mm TC4 titanium alloys billet using die hammer, obtained after cooling
Thickness is 35mm TC4 titanium alloy slabs；Three carried out successively along the three-dimensional of TC4 titanium alloy billets in the multiway forging
Secondary to be unidirectionally forged to one cycle, each deflection unidirectionally forged is 44%；The multiway forging includes 4 and circulated, and the 1st
The initial forging temperature of the secondary circulation is 1050 DEG C, and final forging temperature is 706 DEG C, and the initial forging temperature of the 2nd circulation is 1000 DEG C,
613 DEG C of final forging temperature, the initial forging temperature of the 3rd circulation is 1000 DEG C, 602 DEG C of final forging temperature, the beginning circulated described in the 4th
It is 1000 DEG C to forge temperature, 607 DEG C of final forging temperature；
Annealed Step 2: the TC4 titanium alloy slabs obtained in step 1 are incubated into 30min under conditions of 500 DEG C
Handle, fine grain TC4 titanium alloy plates are obtained after air cooling；
Step 3: the fine grain TC4 titanium alloy plates semi-finished product obtained in step 2 are sheared successively, reconditioning, leveling,
Polishing, polishing and pickling, obtain the fine grain TC4 titanium alloy plates that thickness is 35mm；The temperature of the leveling is 450 DEG C.
After testing, the crystallite dimension of fine grain TC4 titanium alloy plates manufactured in the present embodiment is 1 μm~2 μm.
Embodiment 6 and comparative example 1 are compared to the TC4 titaniums as can be seen that directly using multiway forging method to a diameter of 115mm
Alloy billet is processed, and the crystallite dimension for finally giving sheet material is 1 μm~2 μm, has exceeded the scope of Ultra-fine Grained, has belonged to fine grain
TC4 titanium alloy plates, and use multiway forging method and warm-rolling technique to be processed a diameter of 115mm TC4 titanium alloy billets,
The crystallite dimension for finally giving sheet material is 0.1 μm~0.5 μm, belongs to Ultra-fine Grained TC4 titanium alloy plates, illustrates that warm-rolling technique can be with
The crystal grain of the TC4 titanium alloys after multiway forging is further refined, finally give Ultra-fine Grained TC4 titanium alloy plates.
According to the method in GB/T13810-2007 surgical implant titanium and its alloy works, to embodiment 1~implementation
The room-temperature property of fine grain TC4 titanium alloy plates prepared by medical ultra-fine grain TC4 titanium alloy plates and comparative example 1 prepared by example 6 is entered
Row test, specific data are as shown in table 1.
Prepared by medical ultra-fine grain TC4 titanium alloy plates and comparative example 1 prepared by the 1~embodiment of the embodiment of the present invention 6 of table 1
The performance test data of fine grain TC4 titanium alloy plates
As can be seen from Table 1, the thickness of medical ultra-fine grain TC4 titanium alloy plates prepared by 1~embodiment of the embodiment of the present invention 6
5mm~25mm is spent, crystallite dimension is 0.1 μm~1 μm, and tensile strength Rm at room temperature is 1050MPa~1300MPa, has no progeny and stretches
Long rate is 14%~17%, it is specified that nonproportional cyclic straining RP0.2For 1000MPa~1080MPa, meet GB/T13810-
The regulation of 2007 standards, and the fine grain TC4 titanium alloy plates prepared better than existing product and comparative example 1, illustrate present invention preparation
Medical ultra-fine grain TC4 titanium alloy plate excellent combination properties.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions.It is every according to invention skill
Any simple modification, change and equivalence change that art is substantially made to above example, still fall within technical solution of the present invention
Protection domain in.
Claims (5)
1. a kind of preparation method of medical ultra-fine grain TC4 titanium alloy plates, it is characterised in that this method comprises the following steps：
Step 1: multiway forging is carried out to a diameter of 90mm~410mm TC4 titanium alloys billet using quick forging machine, after cooling
To the TC4 titanium alloy slabs that thickness is 25mm~130mm；In the multiway forging along TC4 titanium alloy billets three-dimensional according to
Secondary progress is unidirectionally forged to one cycle three times, and each deflection unidirectionally forged is 40%~60%；It is described multidirectional
Forging includes 2~4 circulations；The initial forging temperature of 1st circulation is 1050 DEG C~1150 DEG C, and final forging temperature is not less than 700
DEG C, the initial forging temperature circulated described in the 2nd time~the 4th is 700 DEG C~1000 DEG C, and final forging temperature is not less than 600 DEG C；
Step 2: the TC4 titanium alloy slabs obtained in step 1 are first carried out into reconditioning, then made annealing treatment, then at 550 DEG C
Multi-pass warm-rolling is carried out under conditions of~700 DEG C, the TC4 titanium alloy plates that thickness is 6mm~26mm are obtained after air cooling；The temperature
The pass deformation rolled is 10%~20%, and the total deformation of the warm-rolling is not less than 50%；
Step 3: the TC4 titanium alloy plates obtained in step 2 are made annealing treatment, the conjunction of Ultra-fine Grained TC4 titaniums is obtained after air cooling
Golden plate material semi-finished product；
Step 4: the Ultra-fine Grained TC4 titanium alloy plates semi-finished product obtained in step 3 are sheared successively, reconditioning, leveling, mill
Light, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plates that thickness is 5mm~25mm.
A kind of 2. preparation method of medical ultra-fine grain TC4 titanium alloy plates according to claim 1, it is characterised in that step
Quick forging machine described in rapid one is die hammer or hydraulic press.
A kind of 3. preparation method of medical ultra-fine grain TC4 titanium alloy plates according to claim 1, it is characterised in that step
The temperature made annealing treatment described in rapid two is 550 DEG C~700 DEG C, and the time is 60min~80min.
A kind of 4. preparation method of medical ultra-fine grain TC4 titanium alloy plates according to claim 1, it is characterised in that step
The temperature made annealing treatment described in rapid three is 500 DEG C~650 DEG C, and the time is 30min~60min.
A kind of 5. preparation method of medical ultra-fine grain TC4 titanium alloy plates according to claim 1, it is characterised in that step
The temperature of leveling described in rapid four is 400 DEG C~500 DEG C.
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| CN110814246A (en) * | 2019-11-22 | 2020-02-21 | 西安庄信新材料科技有限公司 | Forging process of titanium plate blank |
| CN111014333A (en) * | 2019-12-12 | 2020-04-17 | 西安圣泰金属材料有限公司 | Processing method of medical Ti6Al4V titanium alloy plate |
| CN113481475A (en) * | 2021-07-05 | 2021-10-08 | 宁波江丰电子材料股份有限公司 | Method for refining titanium target material grains and titanium target material |
| CN113564500A (en) * | 2021-06-27 | 2021-10-29 | 中国科学院金属研究所 | Preparation method of high-strength ultrafine-grained TC4 titanium alloy foil |
| CN114150243A (en) * | 2021-11-26 | 2022-03-08 | 中国航发北京航空材料研究院 | Preparation method of ultrafine equiaxial TC4 titanium alloy wire |
| CN114799738A (en) * | 2022-03-24 | 2022-07-29 | 新疆湘润新材料科技有限公司 | Preparation method of TC4 titanium alloy thin-wall ring material |
| CN115786747A (en) * | 2022-11-24 | 2023-03-14 | 西北有色金属研究院 | Preparation method of medical high-performance antibacterial titanium alloy plate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040094241A1 (en) * | 2002-06-21 | 2004-05-20 | Yoji Kosaka | Titanium alloy and automotive exhaust systems thereof |
| US20060225818A1 (en) * | 2005-03-08 | 2006-10-12 | Waldemar Link Gmbh & Co. Kg | Process for casting a beta-titanium alloy |
| CN102943228A (en) * | 2012-12-14 | 2013-02-27 | 西北有色金属研究院 | Machining method for improving obdurability of two-phase titanium alloy large-size bar |
| CN103361586A (en) * | 2013-07-31 | 2013-10-23 | 西北有色金属研究院 | Processing method for raising strength and toughness of TC4-DT titanium alloy sheet materials |
-
2017
- 2017-09-18 CN CN201710841918.2A patent/CN107574394B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040094241A1 (en) * | 2002-06-21 | 2004-05-20 | Yoji Kosaka | Titanium alloy and automotive exhaust systems thereof |
| US20060225818A1 (en) * | 2005-03-08 | 2006-10-12 | Waldemar Link Gmbh & Co. Kg | Process for casting a beta-titanium alloy |
| CN102943228A (en) * | 2012-12-14 | 2013-02-27 | 西北有色金属研究院 | Machining method for improving obdurability of two-phase titanium alloy large-size bar |
| CN103361586A (en) * | 2013-07-31 | 2013-10-23 | 西北有色金属研究院 | Processing method for raising strength and toughness of TC4-DT titanium alloy sheet materials |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108480418A (en) * | 2018-03-19 | 2018-09-04 | 江苏大学 | A kind of preparation method of high intensity TC6 titanium-alloy thin-plates |
| CN110814246A (en) * | 2019-11-22 | 2020-02-21 | 西安庄信新材料科技有限公司 | Forging process of titanium plate blank |
| CN110814246B (en) * | 2019-11-22 | 2021-06-25 | 西安庄信新材料科技有限公司 | Forging process of titanium plate blank |
| CN111014333A (en) * | 2019-12-12 | 2020-04-17 | 西安圣泰金属材料有限公司 | Processing method of medical Ti6Al4V titanium alloy plate |
| CN113564500B (en) * | 2021-06-27 | 2022-08-09 | 中国科学院金属研究所 | Preparation method of high-strength ultrafine-grained TC4 titanium alloy foil |
| CN113564500A (en) * | 2021-06-27 | 2021-10-29 | 中国科学院金属研究所 | Preparation method of high-strength ultrafine-grained TC4 titanium alloy foil |
| CN113481475A (en) * | 2021-07-05 | 2021-10-08 | 宁波江丰电子材料股份有限公司 | Method for refining titanium target material grains and titanium target material |
| CN114150243A (en) * | 2021-11-26 | 2022-03-08 | 中国航发北京航空材料研究院 | Preparation method of ultrafine equiaxial TC4 titanium alloy wire |
| CN114150243B (en) * | 2021-11-26 | 2022-08-19 | 中国航发北京航空材料研究院 | Preparation method of ultrafine equiaxial TC4 titanium alloy wire |
| CN114799738A (en) * | 2022-03-24 | 2022-07-29 | 新疆湘润新材料科技有限公司 | Preparation method of TC4 titanium alloy thin-wall ring material |
| CN114799738B (en) * | 2022-03-24 | 2023-12-22 | 新疆湘润新材料科技有限公司 | Preparation method of TC4 titanium alloy thin-wall ring material |
| CN115786747A (en) * | 2022-11-24 | 2023-03-14 | 西北有色金属研究院 | Preparation method of medical high-performance antibacterial titanium alloy plate |
| CN115786747B (en) * | 2022-11-24 | 2024-01-26 | 西北有色金属研究院 | Preparation method of medical high-performance antibacterial titanium alloy plate |
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