CN107574394B - A kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate - Google Patents

A kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate Download PDF

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CN107574394B
CN107574394B CN201710841918.2A CN201710841918A CN107574394B CN 107574394 B CN107574394 B CN 107574394B CN 201710841918 A CN201710841918 A CN 201710841918A CN 107574394 B CN107574394 B CN 107574394B
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titanium alloy
alloy plate
ultra
temperature
fine grain
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CN107574394A (en
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麻西群
于振涛
皇甫强
张亚峰
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西北有色金属研究院
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Abstract

The present invention provides a kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate, this method comprises: one, multiway forging is carried out to the TC4 titanium alloy billet that diameter is 90mm~410mm, obtain the TC4 titanium alloy slab with a thickness of 25mm~130mm after cooling;Two, TC4 titanium alloy slab is successively subjected to reconditioning, annealing and warm-rolling, the TC4 titanium alloy plate with a thickness of 6mm~26mm is obtained after air-cooled;Three, TC4 titanium alloy plate is made annealing treatment, Ultra-fine Grained TC4 titanium alloy plate semi-finished product is obtained after air-cooled;Four, Ultra-fine Grained TC4 titanium alloy plate semi-finished product are successively sheared, reconditioning, leveling, polishing, polishing and pickling, obtains the Ultra-fine Grained TC4 titanium alloy plate with a thickness of 5mm~25mm.The present invention combines multiway forging technique and warm-rolling technique, and the crystallite dimension for obtaining medical ultra-fine grain TC4 titanium alloy plate is 0.1 μm~1 μm, and surfacing, even tissue, good mechanical properties, meets the regulation of GB/T13810-2007 standard.

Description

A kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate

Technical field

The invention belongs to titanium alloy material processing technique fields, and in particular to a kind of medical ultra-fine grain TC4 titanium alloy plate Preparation method.

Background technique

80% or more titanium alloy raw material are TC4 titanium alloy in medical instrument both at home and abroad at present, are mainly used for making mouth The implantation instruments such as the gear divisions such as chamber corona, fixed bridge, denture class, joint type and wound class.The study found that the property of metal material Can be closely related with its crystallite dimension, when the crystallite dimension of metal refine to 1 μm or less, can get by uniform equiax crystal group The super fine crystal material to occupy the majority at, high-angle boundary, super fine crystal material have high intensity at room temperature, have super modeling under high temperature Property.Ultra-fine Grained TC4 titanium alloy has higher intensity, better fatigue behaviour and stronger compared with common TC4 titanium alloy Corrosion resistance has 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 lower atomic density Intergranular district's groups at, typical sizes of crystalline region or other feature length be at least in one-dimensional direction (0.1 μm of sub-micron ~1 μm)/nanometer (< 100nm).

The forced plasticity deforming method of titanium alloy specifically includes that equal channel angular pressing (ECAP), high pressure and torsion (HPT), tires out Product pack 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 lesser Ultra fine grained steel bar is the main method of industrialized production Ultra-fine Grained titanium, but yield is lower, and to the plasticity of titanium alloy material, Equipment and mold requires high;Accumulation pack rolling method is able to produce the thin plate and foil material of relatively thin size, and accumulates the work of pack rolling method Sequence is complicated, is easy to produce 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 mostly use greatly the titanium alloy plate of smaller size (thickness is less than 90mm) to carry out experimental exploration, And the equipment and moulds of industrial equipment used costly with it is special, the Ultra-fine Grained plate thickness prepared by multiway forging method is 2mm, Length and width are 300mm × 200mm, are not easy to be processed, and rough surface, flatness is poor, and mechanical property is bad, it is difficult to meet doctor It learns and requires.

Summary of the invention

Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of medical ultra-fine grain The preparation method of TC4 titanium alloy plate.This method using diameter for 90mm~410mm TC4 titanium alloy billet as raw material, will be multidirectional Forging technology and warm-rolling technique combine, and the crystallite dimension of the medical ultra-fine grain TC4 titanium alloy plate of preparation is 0.1 μm~1 μm, With a thickness of 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 simple process, it is easy to accomplish, the requirement to equipment is low, can meet The industrial production demand of Ultra-fine Grained TC4 titanium alloy.

In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of medical ultra-fine grain TC4 titanium alloy plate Preparation method, which is characterized in that method includes the following steps:

Step 1: multiway forging is carried out to the TC4 titanium alloy billet that diameter is 90mm~410mm using quick forging machine, it is cooling The TC4 titanium alloy slab with a thickness of 25mm~130mm is obtained afterwards;Along the three-dimensional side of TC4 titanium alloy billet in the multiway forging It is unidirectionally forged to one cycle three times to what is successively carried out, 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 of circulation 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: TC4 titanium alloy slab obtained in step 1 is first carried out reconditioning, then made annealing treatment, is then existed Multi-pass warm-rolling is carried out under conditions of 550 DEG C~700 DEG C, and the TC4 titanium alloy plate with a thickness of 6mm~26mm is obtained after air-cooled; 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: TC4 titanium alloy plate obtained in step 2 is made annealing treatment, Ultra-fine Grained TC4 is obtained after air-cooled Titanium alloy plate semi-finished product;

Step 4: Ultra-fine Grained TC4 titanium alloy plate semi-finished product obtained in step 3 are successively sheared, reconditioning, are rectified Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plate with a thickness of 5mm~25mm.

The preparation method of above-mentioned a kind of medical ultra-fine grain TC4 titanium alloy plate, which is characterized 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 plate, which is characterized 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 plate, which is characterized 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 plate, which is characterized in that rectified described in step 4 Flat temperature is 400 DEG C~500 DEG C.

Compared with the prior art, the present invention has the following advantages:

1, it is combined in the present invention using multiway forging technique and warm-rolling technique, is refined first using multiway forging method The crystallite dimension of TC4 titanium alloy and the growth for inhibiting texture avoid anisotropy, reduce the deformation temperature of TC4 titanium alloy Degree, and best rate of deformation is improved, then by warm-rolling, improve plate flatness under mesophilic condition, while continuing to become Shape refines the crystal grain of TC4 titanium alloy further, final to obtain the medical ultra-fine grain TC4 titanium conjunction that crystallite dimension is 0.1 μm~1 μm Golden plate material, the surfacing of medical ultra-fine grain TC4 titanium alloy plate, even tissue.

2, the present invention using diameter for 90mm~410mm TC4 titanium alloy billet as raw material, be prepared with a thickness of 5mm~ The medical ultra-fine grain TC4 titanium alloy plate of 25mm, expands the size range of raw material, improves the machinability of product, the doctor Tensile strength with Ultra-fine Grained TC4 titanium alloy plate is 1050MPa~1300MPa, it is specified that nonproportional cyclic straining is 1000MPa ~1080MPa, elongation after fracture are 14%~17%, meet the regulation of GB/T13810-2007, and be better than existing product.

3, simple process of the invention, 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 alloy, meets the industrial production demand of medical ultra-fine grain TC4 titanium alloy.

Invention is further described in detail with reference to the accompanying drawings and examples.

Detailed description of the invention

Fig. 1 is the schematic diagram of multiway forging technical process of the present invention.

Fig. 2 is the TEM figure of medical ultra-fine grain TC4 titanium alloy plate prepared by the embodiment of the present invention 1.

Fig. 3 is the TEM figure of medical ultra-fine grain TC4 titanium alloy plate prepared by the embodiment of the present invention 3.

Specific embodiment

Fig. 1 is multiway forging technical process schematic diagram of the present invention, and the expression of filled black arrows direction is unidirectionally forged in figure Three directions (the respectively X-axis, Y-axis and Z-direction of TC4 titanium alloy billet).As seen from Figure 1, the 1st time of multiway forging In cyclic process, the is carried out to the end face of TC4 titanium alloy billet along axis direction, that is, Y direction of TC4 titanium alloy billet first Then forge piece is rotated by 90 ° and carries out second of unidirectional forging along Z-direction, is finally rotated by 90 ° again along X by primary unidirectional forging Axis direction 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 Axis direction carries out unidirectional forging for the first time to forge piece, is then rotated by 90 ° forge piece and carries out second of unidirectional forging along Z-direction It makes, is finally rotated by 90 ° again and carries out the unidirectional forging of third time along the x axis, 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 the following steps are included:

Step 1: carrying out multiway forging to the TC4 titanium alloy billet that diameter is 410mm using hydraulic press, obtained after cooling With a thickness of the TC4 titanium alloy slab of 130mm;What the three-dimensional in the multiway forging along TC4 titanium alloy billet successively carried out It is unidirectionally forged to one cycle three times, 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, circulation described in the 4th Initial forging temperature is 700 DEG C, 617 DEG C of final forging temperature;

Step 2: by after TC4 titanium alloy slab reconditioning obtained in step 1, kept the temperature under conditions of 700 DEG C 80min into Row annealing, three passage warm-rollings are then carried out under conditions of 700 DEG C, the TC4 titanium alloy with a thickness of 26mm is obtained after air-cooled Plate;The pass deformation of the warm-rolling is 20%, and the total deformation of the warm-rolling is 60%;

It anneals Step 3: TC4 titanium alloy plate obtained in step 2 to be kept the temperature to 60min under conditions of 650 DEG C Processing, obtains Ultra-fine Grained TC4 titanium alloy plate semi-finished product after air-cooled;

Step 4: Ultra-fine Grained TC4 titanium alloy plate semi-finished product obtained in step 3 are successively sheared, reconditioning, are rectified Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plate with a thickness of 25mm;The temperature of the leveling is 500℃。

Fig. 2 is that the TEM of medical ultra-fine grain TC4 titanium alloy plate 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 plate of preparation is uniform, and crystallite dimension is 0.5 μm~1 μm.

Embodiment 2

The preparation method of the present embodiment the following steps are included:

Step 1: carrying out multiway forging to the TC4 titanium alloy billet that diameter is 150mm using die hammer, obtained after cooling With a thickness of the TC4 titanium alloy slab of 130mm;What the three-dimensional in the multiway forging along TC4 titanium alloy billet successively carried out It is unidirectionally forged to one cycle three times, 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 TC4 titanium alloy slab reconditioning obtained in step 1, kept the temperature under conditions of 630 DEG C 60min into Row annealing, five passage warm-rollings are then carried out under conditions of 630 DEG C, the TC4 titanium alloy with a thickness of 11mm is obtained after air-cooled Plate;The pass deformation of the warm-rolling is 10%, and the total deformation of the warm-rolling is 50%;

It anneals Step 3: TC4 titanium alloy plate obtained in step 2 to be kept the temperature to 40min under conditions of 550 DEG C Processing, obtains Ultra-fine Grained TC4 titanium alloy plate semi-finished product after air-cooled;

Step 4: Ultra-fine Grained TC4 titanium alloy plate semi-finished product obtained in step 3 are successively sheared, reconditioning, are rectified Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plate with a thickness of 10mm;The temperature of the leveling is 430℃。

Through detecting, the crystallite dimension of medical ultra-fine grain TC4 titanium alloy plate manufactured in the present embodiment is 0.8 μm~1 μm.

Embodiment 3

The preparation method of the present embodiment the following steps are included:

Step 1: carrying out multiway forging to the TC4 titanium alloy billet that diameter is 210mm using hydraulic press, obtained after cooling With a thickness of the TC4 titanium alloy slab of 65mm;Three-dimensional in the multiway forging along TC4 titanium alloy billet successively carry out three Secondary to be unidirectionally forged to one cycle, each deflection unidirectionally forged is 50%;The multiway forging is recycled including 3, 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 TC4 titanium alloy slab reconditioning obtained in step 1, kept the temperature under conditions of 650 DEG C 80min into Row annealing, three passage warm-rollings are then carried out under conditions of 650 DEG C, the TC4 titanium alloy with a thickness of 26mm is obtained after air-cooled Plate;The pass deformation of the warm-rolling is 20%, and the total deformation of the warm-rolling is 60%;

It anneals Step 3: TC4 titanium alloy plate obtained in step 2 to be kept the temperature to 60min under conditions of 600 DEG C Processing, obtains Ultra-fine Grained TC4 titanium alloy plate semi-finished product after air-cooled;

Step 4: Ultra-fine Grained TC4 titanium alloy plate semi-finished product obtained in step 3 are successively sheared, reconditioning, are rectified Flat, polishing, polishing and pickling, obtain with a thickness of 15mm medical ultra-fine grain TC4 titanium alloy plate;The temperature of the leveling is 450 ℃。

Fig. 3 is that the TEM of medical ultra-fine grain TC4 titanium alloy plate manufactured in the present embodiment schemes, this implementation as can be seen from Figure 3 The interior tissue of the medical ultra-fine grain TC4 titanium alloy plate of example preparation is uniform, and crystallite dimension is 0.4 μm~0.6 μm.

Embodiment 4

The preparation method of the present embodiment the following steps are included:

Step 1: carrying out multiway forging to the TC4 titanium alloy billet that diameter is 350mm using hydraulic press, obtained after cooling With a thickness of the TC4 titanium alloy slab of 100mm;What the three-dimensional in the multiway forging along TC4 titanium alloy billet successively carried out It is unidirectionally forged to one cycle three times, 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, circulation described in the 4th Initial forging temperature is 800 DEG C, 619 DEG C of final forging temperature;

Step 2: by after TC4 titanium alloy slab reconditioning obtained in step 1, kept the temperature under conditions of 650 DEG C 70min into Row annealing, three passage warm-rollings are then carried out under conditions of 650 DEG C, the TC4 titanium alloy with a thickness of 21mm is obtained after air-cooled Plate;The pass deformation of the warm-rolling is 20%, and the total deformation of the warm-rolling is 60%;

It anneals Step 3: TC4 titanium alloy plate obtained in step 2 to be kept the temperature to 40min under conditions of 600 DEG C Processing, obtains Ultra-fine Grained TC4 titanium alloy plate semi-finished product after air-cooled;

Step 4: Ultra-fine Grained TC4 titanium alloy plate semi-finished product obtained in step 3 are successively sheared, reconditioning, are rectified Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plate with a thickness of 20mm;The temperature of the leveling is 450℃。

Through detecting, the crystallite dimension of medical ultra-fine grain TC4 titanium alloy plate 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 plate the following steps are included:

Step 1: carrying out multiway forging to the TC4 titanium alloy billet that diameter is 90mm using die hammer, thickness is obtained after cooling Degree is the TC4 titanium alloy slab of 25mm;Three-dimensional in the multiway forging along TC4 titanium alloy billet successively carries out three times It unidirectionally is forged to one cycle, each deflection unidirectionally forged is 40%;The multiway forging is recycled including 2, and 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 600 DEG C of temperature of forging;

Step 2: by after TC4 titanium alloy slab reconditioning obtained in step 1, kept the temperature under conditions of 550 DEG C 60min into Row annealing, four-pass warm-rolling is then carried out under conditions of 550 DEG C, the TC4 titanium alloy sheet with a thickness of 6mm is obtained after air-cooled Material;The pass deformation of the warm-rolling is 15%, and the total deformation of the warm-rolling is 60%;

It anneals Step 3: TC4 titanium alloy plate obtained in step 2 to be kept the temperature to 30min under conditions of 500 DEG C Processing, obtains Ultra-fine Grained TC4 titanium alloy plate semi-finished product after air-cooled;

Step 4: Ultra-fine Grained TC4 titanium alloy plate semi-finished product obtained in step 3 are successively sheared, reconditioning, are rectified Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plate with a thickness of 5mm;The temperature of the leveling is 400 ℃。

Through detecting, the crystallite dimension of medical ultra-fine grain TC4 titanium alloy plate manufactured in the present embodiment is 0.7 μm~0.9 μm.

Embodiment 6

The preparation method of the present embodiment the following steps are included:

Step 1: carrying out multiway forging to the TC4 titanium alloy billet that diameter is 115mm using die hammer, obtained after cooling With a thickness of the TC4 titanium alloy slab of 35mm;Three-dimensional in the multiway forging along TC4 titanium alloy billet successively carry out three Secondary to be unidirectionally forged to one cycle, each deflection unidirectionally forged is 44%;The multiway forging is recycled including 4, 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 of circulation described in the 4th Forging temperature is 1000 DEG C, 607 DEG C of final forging temperature;

Step 2: by after TC4 titanium alloy slab reconditioning obtained in step 1, kept the temperature under conditions of 600 DEG C 60min into Row annealing, warm-rolling is then carried out under conditions of 600 DEG C, the TC4 titanium alloy plate with a thickness of 7mm is obtained after air-cooled;Institute The pass deformation for stating warm-rolling is 16%, and the total deformation of the warm-rolling is 80%;

It anneals Step 3: TC4 titanium alloy plate obtained in step 2 to be kept the temperature to 30min under conditions of 500 DEG C Processing, obtains Ultra-fine Grained TC4 titanium alloy plate semi-finished product after air-cooled;

Step 4: Ultra-fine Grained TC4 titanium alloy plate semi-finished product obtained in step 3 are successively sheared, reconditioning, are rectified Flat, polishing, polishing and pickling, obtain the medical ultra-fine grain TC4 titanium alloy plate with a thickness of 5mm;The temperature of the leveling is 450 ℃。

Through detecting, the crystallite dimension of medical ultra-fine grain TC4 titanium alloy plate manufactured in the present embodiment is 0.1 μm~0.5 μm.

Comparative example 1

The preparation method of this comparative example the following steps are included:

Step 1: carrying out multiway forging to the TC4 titanium alloy billet that diameter is 115mm using die hammer, obtained after cooling With a thickness of the TC4 titanium alloy slab of 35mm;Three-dimensional in the multiway forging along TC4 titanium alloy billet successively carry out three Secondary to be unidirectionally forged to one cycle, each deflection unidirectionally forged is 44%;The multiway forging is recycled including 4, 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 of circulation described in the 4th Forging temperature is 1000 DEG C, 607 DEG C of final forging temperature;

It anneals Step 2: TC4 titanium alloy slab obtained in step 1 to be kept the temperature to 30min under conditions of 500 DEG C Processing, obtains fine grain TC4 titanium alloy plate after air-cooled;

Step 3: fine grain TC4 titanium alloy plate semi-finished product obtained in step 2 are successively sheared, reconditioning, leveling, Polishing, polishing and pickling, obtain the fine grain TC4 titanium alloy plate with a thickness of 35mm;The temperature of the leveling is 450 DEG C.

Through detecting, the crystallite dimension of fine grain TC4 titanium alloy plate manufactured in the present embodiment is 1 μm~2 μm.

Embodiment 6 and comparative example 1 are compared as can be seen that directlying adopt the TC4 titanium that multiway forging method is 115mm to diameter Alloy billet is processed, and the crystallite dimension for finally obtaining plate is 1 μm~2 μm, has been more than the range of Ultra-fine Grained, has been belonged to fine grain TC4 titanium alloy plate, and multiway forging method and warm-rolling technique is used to process diameter for the TC4 titanium alloy billet of 115mm, The crystallite dimension for finally obtaining plate is 0.1 μm~0.5 μm, belongs to Ultra-fine Grained TC4 titanium alloy plate, illustrates that warm-rolling technique can be with The crystal grain of TC4 titanium alloy after making multiway forging further refines, and finally obtains Ultra-fine Grained TC4 titanium alloy plate.

According to the method in GB/T13810-2007 surgical implant titanium and its alloy work, to embodiment 1~implementation Example 6 prepare medical ultra-fine grain TC4 titanium alloy plate and comparative example 1 prepare fine grain TC4 titanium alloy plate room-temperature property into Row test, specific data are as shown in table 1.

Prepared by the medical ultra-fine grain TC4 titanium alloy plate and comparative example 1 of 1 1~embodiment of the embodiment of the present invention 6 of table preparation The performance test data of fine grain TC4 titanium alloy plate

As can be seen from Table 1, the thickness for the medical ultra-fine grain TC4 titanium alloy plate that 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 plate prepared better than existing product and comparative example 1, illustrate preparation of the present invention Medical ultra-fine grain TC4 titanium alloy plate excellent combination property.

The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention Protection scope in.

Claims (4)

1. a kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate, which is characterized in that method includes the following steps:
Step 1: multiway forging is carried out to the TC4 titanium alloy billet that diameter is 90mm~410mm using die hammer or hydraulic press, The TC4 titanium alloy slab with a thickness of 25mm~130mm is obtained after cooling;Along the three of TC4 titanium alloy billet in the multiway forging What dimension direction successively carried out is unidirectionally forged to one cycle three times, and each deflection unidirectionally forged is 40%~60%; The 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 Lower than 700 DEG C, the initial forging temperature of circulation described in the 2nd time~the 4th is 700 DEG C~1000 DEG C, and final forging temperature is not less than 600 ℃;
Step 2: TC4 titanium alloy slab obtained in step 1 is first carried out reconditioning, then made annealing treatment, then at 550 DEG C Multi-pass warm-rolling is carried out under conditions of~700 DEG C, and the TC4 titanium alloy plate with a thickness of 6mm~26mm is obtained after air-cooled;The temperature The pass deformation rolled is 10%~20%, and the total deformation of the warm-rolling is not less than 50%;
Step 3: TC4 titanium alloy plate obtained in step 2 is made annealing treatment, the conjunction of Ultra-fine Grained TC4 titanium is obtained after air-cooled Golden plate material semi-finished product;
Step 4: Ultra-fine Grained TC4 titanium alloy plate semi-finished product obtained in step 3 are successively sheared, reconditioning, leveling, mill Light, polishing and pickling obtain the medical ultra-fine grain TC4 titanium alloy plate with a thickness of 5mm~25mm.
2. a kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate according to claim 1, which is characterized in that step The temperature of annealing described in rapid two is 550 DEG C~700 DEG C, and the time is 60min~80min.
3. a kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate according to claim 1, which is characterized in that step The temperature of annealing described in rapid three is 500 DEG C~650 DEG C, and the time is 30min~60min.
4. a kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate according to claim 1, which is characterized in that step The temperature of leveling described in rapid four is 400 DEG C~500 DEG C.
CN201710841918.2A 2017-09-18 2017-09-18 A kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate CN107574394B (en)

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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

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