CN107574394A - A kind of preparation method of medical ultra-fine grain TC4 titanium alloy plates - Google Patents

Abstract

The invention provides a method for preparing medical ultra-fine-grained TC4 titanium alloy plate. The method comprises: 1. Carrying out multidirectional forging to a TC4 titanium alloy round ingot with a diameter of 90 mm to 410 mm, and cooling to obtain a TC4 titanium alloy plate with a thickness of 25 mm to 130 mm. TC4 titanium alloy slab; 2. The TC4 titanium alloy slab is ground, annealed and warm-rolled in sequence, and after air cooling, a TC4 titanium alloy plate with a thickness of 6mm to 26mm is obtained; 3. The TC4 titanium alloy plate is annealed, air-cooled Finally, the semi-finished product of ultra-fine-grained TC4 titanium alloy plate is obtained; 4. The semi-finished product of ultra-fine-grained TC4 titanium alloy plate is successively cut, ground, leveled, polished, polished and pickled to obtain ultra-fine-grained TC4 titanium alloy plate with a thickness of 5mm to 25mm. Crystal TC4 titanium alloy plate. The invention combines the multi-directional forging process and the warm rolling process to obtain the medical ultra-fine-grained TC4 titanium alloy plate with a grain size of 0.1 μm to 1 μm, smooth surface, uniform structure, good mechanical properties, and conforms to GB/T13810‑2007 Standard provisions.

Description

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

technical field

The invention belongs to the technical field of titanium alloy material processing, and in particular relates to a preparation method of a medical ultrafine-grained TC4 titanium alloy plate.

Background technique

At present, more than 80% of the titanium alloy raw materials in domestic and foreign medical devices are TC4 titanium alloys, which are mainly used to make dental, joint and trauma implants such as dental crowns, fixed bridges, and denture brackets. Research has found that the properties of metal materials are closely related to their grain size. When the grain size of the metal is refined to less than 1 μm, an ultra-fine-grained material composed of uniform equiaxed grains and large-angle grain boundaries can be obtained. Crystalline materials have high strength at room temperature and superplasticity at high temperatures. Compared with ordinary TC4 titanium alloy, ultra-fine-grained TC4 titanium alloy has higher strength, better fatigue performance and stronger corrosion resistance, and has broad application prospects in the field of medical materials.

The strong plastic deformation method is recognized by the international materials community as the most promising method for preparing bulk ultrafine-grained materials. It can refine the grains of coarse-grained metals to the nanometer level, and the prepared ultrafine-grained materials The typical size of its crystal region or other characteristic length is submicron (0.1 μm ~ 1 μm) / nanometer (<100nm) in at least one dimension.

The strong plastic deformation methods of titanium alloy mainly include: equal channel angular extrusion method (ECAP), high pressure torsion method (HPT), cumulative rolling method (ARB) and multidirectional forging method (MF). The equal channel angle method and the high-pressure torsion method can be used to prepare ultra-fine-grained rods with small three-dimensional dimensions. The requirements are extremely high; the cumulative stack rolling method can produce thinner sheets and foil strips, and the cumulative stack rolling method is complex and prone to wrapping waste; the multi-directional forging method deforms the titanium alloy from different directions to achieve For the purpose of refining grains and improving material properties, most of the titanium alloy plates with smaller sizes (thickness less than 90mm) are used for experiments and exploration, and the equipment and tooling molds used are relatively expensive and special. The thickness of the crystal plate is 2mm, the length and width are 300mm×200mm, it is not easy to process, and the surface is rough, the flatness is poor, the mechanical properties are not good, and it is difficult to meet the medical requirements.

Contents of the invention

The technical problem to be solved by the present invention is to provide a method for preparing medical ultrafine-grained TC4 titanium alloy plate aiming at the deficiencies of the above-mentioned prior art. The method uses TC4 titanium alloy round ingots with a diameter of 90 mm to 410 mm as raw materials, combines the multi-directional forging process and the warm rolling process, and prepares medical ultra-fine-grained TC4 titanium alloy plates with a grain size of 0.1 μm to 1 μm and a thickness of 0.1 μm to 1 μm. The tensile strength is 5mm-25mm, the tensile strength is 1050MPa-1300MPa, the specified non-proportional elongation strength is 1000MPa-1080MPa, and the elongation after fracture is 14%-17%. The industrial production demand of ultra-fine grain TC4 titanium alloy.

In order to solve the above-mentioned technical problems, the technical solution adopted in the present invention is: a kind of preparation method of medical ultra-fine grain TC4 titanium alloy plate, it is characterized in that, this method comprises the following steps:

Step 1. Use a fast forging machine to carry out multidirectional forging on a TC4 titanium alloy round ingot with a diameter of 90 mm to 410 mm, and obtain a TC4 titanium alloy slab with a thickness of 25 mm to 130 mm after cooling; The three unidirectional forgings in the three-dimensional direction of the ingot are one cycle, and the deformation of the unidirectional forging is 40% to 60% each time; the multidirectional forging includes 2 to 4 cycles; the first cycle The initial forging temperature is 1050℃～1150℃, the final forging temperature is not lower than 700℃, the initial forging temperature of the second to fourth cycle is 700℃～1000℃, and the final forging temperature is not lower than 600℃. ℃;

Step 2: Grind the TC4 titanium alloy slab obtained in step 1 first, then perform annealing treatment, then perform multi-pass warm rolling under the condition of 550°C-700°C, and obtain a slab with a thickness of 6mm-26mm after air cooling TC4 titanium alloy plate; the deformation of the warm rolling pass is 10% to 20%, and the total deformation of the warm rolling is not less than 50%;

Step 3, annealing the TC4 titanium alloy plate obtained in step 2, and obtaining an ultra-fine-grained TC4 titanium alloy plate semi-finished product after air cooling;

Step 4: Cutting, grinding, leveling, polishing, polishing and pickling the semi-finished ultra-fine-grained TC4 titanium alloy plate obtained in step 3 in sequence to obtain a medical ultra-fine-grained TC4 titanium alloy with a thickness of 5 mm to 25 mm sheet.

The above-mentioned method for preparing a medical ultra-fine-grained TC4 titanium alloy plate is characterized in that the fast forging machine described in step 1 is a die forging hammer or a hydraulic press.

The above-mentioned method for preparing a medical ultrafine-grained TC4 titanium alloy plate is characterized in that the temperature of the annealing treatment in step 2 is 550° C. to 700° C., and the time is 60 minutes to 80 minutes.

The above-mentioned method for preparing a medical ultrafine-grained TC4 titanium alloy plate is characterized in that the temperature of the annealing treatment in step 3 is 500° C. to 650° C., and the time is 30 minutes to 60 minutes.

The above-mentioned method for preparing a medical ultra-fine-grained TC4 titanium alloy plate is characterized in that the temperature for leveling in Step 4 is 400°C-500°C.

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

1. In the present invention, the combination of multi-directional forging process and warm rolling process is adopted. Firstly, the multi-directional forging method is used to refine the grain size of TC4 titanium alloy and inhibit the growth of texture, so as to avoid anisotropy and reduce the TC4 titanium The deformation temperature of the alloy is increased, and the optimal deformation rate is increased, and then the flatness of the plate is improved under medium temperature conditions through warm rolling, and at the same time, deformation is continued to further refine the grains of the TC4 titanium alloy, and finally the grain size is 0.1μm~ 1 μm medical ultra-fine-grained TC4 titanium alloy plate, the medical ultra-fine-grained TC4 titanium alloy plate has a flat surface and a uniform structure.

2. The present invention uses TC4 titanium alloy round ingots with a diameter of 90 mm to 410 mm as raw materials to prepare medical ultrafine-grained TC4 titanium alloy plates with a thickness of 5 mm to 25 mm, which expands the size range of raw materials and improves the machinability of products , the tensile strength of the medical ultra-fine-grained TC4 titanium alloy plate is 1050MPa-1300MPa, the specified non-proportional elongation strength is 1000MPa-1080MPa, and the elongation after fracture is 14%-17%, which meets the requirements of GB/T13810-2007, and superior to existing products.

3. The process of the present invention is simple, easy to implement, and has low requirements for equipment. The preparation of medical ultra-fine-grained TC4 titanium alloy can be realized on ordinary fast forging machines and rolling mills, meeting the industrial production requirements of medical ultra-fine-grained TC4 titanium alloys .

The present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments.

Description of drawings

Fig. 1 is a schematic diagram of the multidirectional forging process of the present invention.

Fig. 2 is a TEM image of the medical ultra-fine-grained TC4 titanium alloy sheet prepared in Example 1 of the present invention.

Fig. 3 is a TEM image of the medical ultra-fine-grained TC4 titanium alloy sheet prepared in Example 3 of the present invention.

detailed description

Fig. 1 is a schematic diagram of the multidirectional forging process of the present invention, in which the directions of solid black arrows represent three directions of unidirectional forging (respectively the X-axis, Y-axis and Z-axis directions of the TC4 titanium alloy round ingot). It can be seen from Figure 1 that in the first cycle of multi-directional forging, the first unidirectional forging is performed on the end face of the TC4 titanium alloy round ingot along the axis direction of the TC4 titanium alloy round ingot, that is, the Y-axis direction, and then the The forging is rotated 90° for the second unidirectional forging along the Z-axis, and finally rotated 90° for the third unidirectional forging along the X-axis to complete the first cycle; the second to fourth times of multi-directional forging In the cycle process, the forging is firstly forged along the Y-axis for the first time, then the forging is rotated 90° for the second one-way along the Z-axis, and finally rotated 90° for the second time along the X-axis. Three times of one-way forging completes a single cycle, and repeats a single cycle to complete the second to fourth cycles of multi-directional forging.

Example 1

The preparation method of the present embodiment comprises the following steps:

Step 1, using a hydraulic press to carry out multi-directional forging on a TC4 titanium alloy round ingot with a diameter of 410 mm, and obtain a TC4 titanium alloy slab with a thickness of 130 mm after cooling; the multi-directional forging is carried out sequentially along the three-dimensional direction of the TC4 titanium alloy round ingot The three unidirectional forgings are one cycle, and the deformation of the unidirectional forging is 60% each time; the multi-directional forging includes 4 cycles, the initial forging temperature of the first cycle is 1150 ° C, and the final forging temperature is 715°C, the initial forging temperature of the second cycle is 950°C, the final forging temperature is 602°C, the initial forging temperature of the third cycle is 800°C, and the final forging temperature is 610°C, the fourth cycle The initial forging temperature is 700°C, and the final forging temperature is 617°C;

Step 2. After grinding the TC4 titanium alloy slab obtained in step 1, heat it at 700°C for 80 minutes for annealing treatment, then carry out three passes of warm rolling at 700°C, and air-cool to obtain a thickness of 26mm. TC4 titanium alloy plate; the pass deformation of the warm rolling is 20%, and the total deformation of the warm rolling is 60%;

Step 3, heat the TC4 titanium alloy sheet material obtained in step 2 for 60 minutes under the condition of 650 ° C for annealing treatment, and obtain an ultra-fine-grained TC4 titanium alloy sheet material semi-finished product after air cooling;

Step 4: Cutting, grinding, leveling, polishing, polishing and pickling the semi-finished ultra-fine-grained TC4 titanium alloy plate obtained in step 3 in sequence to obtain a medical ultra-fine-grained TC4 titanium alloy plate with a thickness of 25 mm; The leveling temperature is 500°C.

Fig. 2 is the TEM picture of the medical ultra-fine grain TC4 titanium alloy sheet material prepared by the present embodiment, as can be seen from Fig. 2 the internal structure of the medical ultrafine grain TC4 titanium alloy sheet material prepared by the embodiment is uniform, and the grain size is 0.5 μm～ 1 μm.

Example 2

The preparation method of the present embodiment comprises the following steps:

Step 1, using a die forging hammer to carry out multidirectional forging to a TC4 titanium alloy round ingot with a diameter of 150 mm, and obtain a TC4 titanium alloy slab with a thickness of 130 mm after cooling; in the multidirectional forging, follow the three-dimensional direction of the TC4 titanium alloy round ingot Three successive unidirectional forgings constitute one cycle, and the deformation of each said unidirectional forging is 45%. The temperature is 700°C, the initial forging temperature of the second cycle is 900°C, and the final forging temperature is 634°C;

Step 2. After grinding the TC4 titanium alloy slab obtained in step 1, heat it at 630°C for 60 minutes for annealing treatment, then carry out five passes of warm rolling at 630°C, and air-cool to obtain a thickness of 11mm TC4 titanium alloy plate; the pass deformation of the warm rolling is 10%, and the total deformation of the warm rolling is 50%;

Step 3, heat the TC4 titanium alloy plate obtained in step 2 for 40 minutes at 550° C. for annealing treatment, and obtain an ultra-fine-grained TC4 titanium alloy plate semi-finished product after air cooling;

Step 4: Cutting, grinding, leveling, polishing, polishing and pickling the semi-finished ultra-fine-grained TC4 titanium alloy plate obtained in step 3 in sequence to obtain a medical ultra-fine-grained TC4 titanium alloy plate with a thickness of 10 mm; The leveling temperature is 430°C.

After testing, the grain size of the medical ultra-fine-grained TC4 titanium alloy plate prepared in this embodiment is 0.8 μm-1 μm.

Example 3

The preparation method of the present embodiment comprises the following steps:

Step 1, using a hydraulic press to carry out multi-directional forging on a TC4 titanium alloy round ingot with a diameter of 210 mm, and obtain a TC4 titanium alloy slab with a thickness of 65 mm after cooling; the multi-directional forging is carried out sequentially along the three-dimensional direction of the TC4 titanium alloy round ingot The three unidirectional forgings are one cycle, and the deformation of the unidirectional forging is 50% each time; the multi-directional forging includes 3 cycles, the initial forging temperature of the first cycle is 1050 ° C, and the final forging temperature is 718°C, the initial forging temperature of the second cycle is 950°C, the final forging temperature is 615°C, the initial forging temperature of the third cycle is 700°C, and the final forging temperature is 600°C;

Step 2. After grinding the TC4 titanium alloy slab obtained in step 1, heat it at 650°C for 80 minutes for annealing treatment, then carry out three passes of warm rolling at 650°C, and air-cool to obtain a thickness of 26mm. TC4 titanium alloy plate; the pass deformation of the warm rolling is 20%, and the total deformation of the warm rolling is 60%;

Step 3, heat the TC4 titanium alloy plate obtained in step 2 for 60 minutes at 600° C. for annealing treatment, and obtain an ultra-fine-grained TC4 titanium alloy plate semi-finished product after air cooling;

Step 4: Cutting, grinding, leveling, polishing, polishing and pickling the semi-finished ultra-fine-grained TC4 titanium alloy plate obtained in step 3 in sequence to obtain a medical ultra-fine-grained TC4 titanium alloy plate with a thickness of 15 mm; The above-mentioned leveling temperature is 450°C.

Fig. 3 is the TEM picture of the medical ultra-fine grain TC4 titanium alloy sheet material prepared in this embodiment, as can be seen from Fig. 3 the internal structure of the medical ultrafine grain TC4 titanium alloy sheet material prepared in this embodiment is uniform, and the grain size is 0.4 μm ~0.6 μm.

Example 4

The preparation method of the present embodiment comprises the following steps:

Step 1, using a hydraulic press to carry out multi-directional forging on a TC4 titanium alloy round ingot with a diameter of 350 mm, and obtain a TC4 titanium alloy slab with a thickness of 100 mm after cooling; in the multi-directional forging, proceed sequentially along the three-dimensional direction of the TC4 titanium alloy round ingot The three unidirectional forgings are one cycle, and the deformation amount of the unidirectional forging is 55% each time; the multi-directional forging includes 4 cycles, the initial forging temperature of the first cycle is 1100 ° C, and the final forging temperature is 706°C, the initial forging temperature of the second cycle is 900°C, the final forging temperature is 612°C, the initial forging temperature of the third cycle is 850°C, and the final forging temperature is 607°C, the fourth cycle The initial forging temperature is 800°C, and the final forging temperature is 619°C;

Step 2. After grinding the TC4 titanium alloy slab obtained in step 1, heat it at 650°C for 70 minutes for annealing treatment, then carry out three passes of warm rolling at 650°C, and air-cool to obtain a thickness of 21mm TC4 titanium alloy plate; the pass deformation of the warm rolling is 20%, and the total deformation of the warm rolling is 60%;

Step 3, heat the TC4 titanium alloy plate obtained in step 2 for 40 minutes at 600° C. for annealing treatment, and obtain an ultra-fine-grained TC4 titanium alloy plate semi-finished product after air cooling;

Step 4: Cutting, grinding, leveling, polishing, polishing and pickling the semi-finished ultra-fine-grained TC4 titanium alloy plate obtained in step 3 in sequence to obtain a medical ultra-fine-grained TC4 titanium alloy plate with a thickness of 20 mm; The leveling temperature is 450°C.

After testing, the grain size of the medical ultra-fine-grained TC4 titanium alloy plate prepared in this embodiment is 0.6 μm-0.8 μm.

Example 5

The preparation method of the ultra-fine grain TC4 titanium alloy plate of the present embodiment comprises the following steps:

Step 1, using a die forging hammer to carry out multi-directional forging to a TC4 titanium alloy round ingot with a diameter of 90 mm, and obtain a TC4 titanium alloy slab with a thickness of 25 mm after cooling; in the multi-directional forging, follow the three-dimensional direction of the TC4 titanium alloy round ingot The three unidirectional forgings performed in sequence constitute one cycle, and the deformation amount of each said unidirectional forging is 40%; the multidirectional forging includes 2 cycles, the initial forging temperature of the first cycle is 1050°C, and the final forging The temperature is 719°C, the initial forging temperature of the second cycle is 700°C, and the final forging temperature is 600°C;

Step 2. After grinding the TC4 titanium alloy slab obtained in step 1, heat it at 550°C for 60 minutes for annealing treatment, then carry out four passes of warm rolling at 550°C, and air-cool to obtain a thickness of 6mm. TC4 titanium alloy plate; the pass deformation of the warm rolling is 15%, and the total deformation of the warm rolling is 60%;

Step 3, heat the TC4 titanium alloy sheet material obtained in step 2 for 30 minutes under the condition of 500 ° C for annealing treatment, and obtain an ultra-fine-grained TC4 titanium alloy sheet material semi-finished product after air cooling;

Step 4. Cutting, grinding, leveling, polishing, polishing and pickling the semi-finished ultra-fine-grained TC4 titanium alloy plate obtained in step 3 in sequence to obtain a medical ultra-fine-grained TC4 titanium alloy plate with a thickness of 5 mm; The leveling temperature is 400°C.

After testing, the grain size of the medical ultra-fine-grained TC4 titanium alloy plate prepared in this embodiment is 0.7 μm-0.9 μm.

Example 6

The preparation method of the present embodiment comprises the following steps:

Step 1, using a die forging hammer to carry out multidirectional forging to a TC4 titanium alloy round ingot with a diameter of 115mm, and obtain a TC4 titanium alloy slab with a thickness of 35mm after cooling; in the multidirectional forging, follow the three-dimensional direction of the TC4 titanium alloy round ingot The three unidirectional forgings performed in sequence constitute one cycle, and the deformation of each said unidirectional forging is 44%; the multidirectional forging includes 4 cycles, the initial forging temperature of the first cycle is 1050°C, and the final forging The temperature is 706°C, the initial forging temperature of the second cycle is 1000°C, and the final forging temperature is 613°C, the initial forging temperature of the third cycle is 1000°C, and the final forging temperature is 602°C, and the fourth cycle The initial forging temperature of the cycle is 1000°C, and the final forging temperature is 607°C;

Step 2. After grinding the TC4 titanium alloy slab obtained in step 1, heat it at 600°C for 60 minutes for annealing treatment, then carry out warm rolling at 600°C, and obtain TC4 titanium with a thickness of 7mm after air cooling Alloy plate; the pass deformation of the warm rolling is 16%, and the total deformation of the warm rolling is 80%;

Step 3, heat the TC4 titanium alloy sheet material obtained in step 2 for 30 minutes under the condition of 500 ° C for annealing treatment, and obtain an ultra-fine-grained TC4 titanium alloy sheet material semi-finished product after air cooling;

Step 4. Cutting, grinding, leveling, polishing, polishing and pickling the semi-finished ultra-fine-grained TC4 titanium alloy plate obtained in step 3 in sequence to obtain a medical ultra-fine-grained TC4 titanium alloy plate with a thickness of 5 mm; The leveling temperature is 450°C.

After testing, the grain size of the medical ultra-fine-grained TC4 titanium alloy plate prepared in this embodiment is 0.1 μm-0.5 μm.

Comparative example 1

The preparation method of this comparative example comprises the following steps:

Step 1, using a die forging hammer to carry out multidirectional forging to a TC4 titanium alloy round ingot with a diameter of 115mm, and obtain a TC4 titanium alloy slab with a thickness of 35mm after cooling; in the multidirectional forging, follow the three-dimensional direction of the TC4 titanium alloy round ingot The three unidirectional forgings performed in sequence constitute one cycle, and the deformation of each said unidirectional forging is 44%; the multidirectional forging includes 4 cycles, the initial forging temperature of the first cycle is 1050°C, and the final forging The temperature is 706°C, the initial forging temperature of the second cycle is 1000°C, and the final forging temperature is 613°C, the initial forging temperature of the third cycle is 1000°C, and the final forging temperature is 602°C, and the fourth cycle The initial forging temperature of the cycle is 1000°C, and the final forging temperature is 607°C;

Step 2, heat the TC4 titanium alloy slab obtained in step 1 for 30 minutes under the condition of 500 ° C for annealing, and obtain a fine-grained TC4 titanium alloy plate after air cooling;

Step 3, the fine-grained TC4 titanium alloy plate semi-finished product obtained in step 2 is successively sheared, repaired, leveled, polished, polished and pickled to obtain a fine-grained TC4 titanium alloy plate with a thickness of 35 mm; The flat temperature is 450°C.

After testing, the grain size of the fine-grained TC4 titanium alloy plate prepared in this embodiment is 1 μm-2 μm.

Comparing Example 6 with Comparative Example 1, it can be seen that the TC4 titanium alloy round ingot with a diameter of 115 mm is directly processed by the multi-directional forging method, and the grain size of the finally obtained plate is 1 μm to 2 μm, exceeding the ultrafine grain size. It belongs to the fine-grained TC4 titanium alloy plate, and the TC4 titanium alloy round ingot with a diameter of 115mm is processed by the multi-directional forging method and the warm rolling process, and the grain size of the finally obtained plate is 0.1μm～0.5μm, which belongs to the superfine Crystalline TC4 titanium alloy sheet, indicating that the warm rolling process can further refine the grains of TC4 titanium alloy after multi-directional forging, and finally obtain ultra-fine-grained TC4 titanium alloy sheet.

According to the method in the processing of titanium and titanium alloys for surgical implants in GB/T13810-2007, the medical ultrafine-grained TC4 titanium alloy plates prepared in Examples 1 to 6 and the fine-grained TC4 titanium alloy plates prepared in Comparative Example 1 The room temperature performance was tested, and the specific data are shown in Table 1.

Table 1 Performance test data of the medical ultra-fine-grained TC4 titanium alloy sheet prepared in Examples 1 to 6 of the present invention and the fine-grained TC4 titanium alloy sheet prepared in Comparative Example 1

As can be seen from Table 1, the thickness of the medical ultra-fine-grained TC4 titanium alloy plate prepared in Examples 1 to 6 of the present invention is 5 mm to 25 mm, the grain size is 0.1 μm to 1 μm, and the tensile strength Rm at room temperature is 1050 MPa ~1300MPa, the elongation after fracture is 14%~17%, and the specified non-proportional elongation R _P0.2 is 1000MPa~1080MPa, all of which meet the requirements of the GB/T13810-2007 standard, and are better than the existing products and the preparation of Comparative Example 1 The fine-grained TC4 titanium alloy sheet shows that the medical ultra-fine-grained TC4 titanium alloy sheet prepared by the present invention has excellent comprehensive properties.

The above descriptions are only preferred embodiments of the present invention, and do not limit the present invention in any way. All simple modifications, changes and equivalent changes made to the above embodiments according to the technical essence of the invention still belong to the protection scope of the technical solution of the invention.

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.