CN103436831B - Preparation method for titanium alloy bar for surgical implants - Google Patents
Preparation method for titanium alloy bar for surgical implants Download PDFInfo
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- CN103436831B CN103436831B CN201310360588.7A CN201310360588A CN103436831B CN 103436831 B CN103436831 B CN 103436831B CN 201310360588 A CN201310360588 A CN 201310360588A CN 103436831 B CN103436831 B CN 103436831B
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Abstract
The invention discloses a preparation method for a titanium alloy bar for surgical implants, which is obtained by the following steps: preparing a blank, cogging and forging, performing deformation process, performing annealing treatment, thermally straightening, performing finishing treatment, and performing secondary polishing. The preparation method of the titanium alloy bar for the surgical implants, disclosed in the invention, improves the quality and performance of the titanium alloy bar by means of three-time straightening and three-time annealing treatments, and can meet the export requirements. Besides, after being subjected to heating and heat preservation, a titanium alloy ingot is hammered by hammering equipment till the deformation rate of the ingot reaches 50%-60% and then subjected to compression and drawing for 6-9 times, so that the compactness of the titanium alloy is improved. Furthermore, the temperatures in the processes of the forging and rolling a product in the middle stage are both lower than the phase transition point of 970 DEG C of the titanium alloy, so that the performance and a metallurgical structure of the titanium alloy bar are ensured.
Description
Technical field
The invention belongs to titanium alloy technical field, relate to a kind of preparation method of Titanium Alloys for Surgical Implants bar.
Background technology
Titanium Alloys for Surgical Implants is with the biocompatibility of its excellence, corrosion resisting property and comprehensive mechanical property, be widely used in making multiple orthopaedics, Stomatological Department medicine equipment, as joint prosthesis (Kua, knee, shoulder, ankle, elbow, wrist, articulations digitorum manus etc.), the bone implanted product such as bone wound product (intramedullary nail, steel plate, screw etc.), backbone correcting internal fixation system, and mouth cavity orthodontic product (bracket, band, rescue arch wire, anchorage planting body).
The technique that the preparation method of existing Titanium Alloys for Surgical Implants bar commonly uses is batching preparation-cogging forging-cutting-deformation processing-anneal-hot straightening-turning-finishing process, this preparation method mainly through once align, an anneal, the quality and performance preparing titanium alloy rod bar is poor, do not reach export standard, and its degree of compactness does not reach medical standard.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Titanium Alloys for Surgical Implants bar, solve the problem that the poor and degree of compactness of titanium alloy rod bar quality and performance that existing method prepares does not reach medical standard.
The technical solution adopted in the present invention is, the preparation method of Titanium Alloys for Surgical Implants bar, specifically implements according to following steps:
Step 1, blank prepares
Select the titanium alloy ingot meeting GB/T13810-2007 standard-required as blank, excise the part determining existing defects after UT (Ultrasonic Testing), be then divided into lathe chamfering on segment;
Step 2, cogging is forged
Make its deformation rate reach 50 ~ 60% by after titanium alloy ingot heating and thermal insulation with hammering equipment, then carrying out being cut into finished product bar after pier pulls out 6 ~ 9 times needs the little titanium alloy briquet of weight;
Step 3, deformation processing
Little titanium alloy briquet step 2 obtained is heated to 930 DEG C ~ 960 DEG C after carrying out reconditioning (crackle and defect are fallen in reconditioning) and is incubated 1.5 ~ 2h in resistance furnace, then reconditioning again after ф 50 ~ ф 60 pole is broken into 1 ton of air hammer, in resistance furnace, be heated to 930 DEG C ~ 960 DEG C again and roll equipment with wire rod after being incubated 1 ~ 1.5h make its deformation rate reach 50% ~ 60%, make titanium alloy rod bar;
Step 4, anneal
Titanium alloy rod bar step 3 made is heated to 680 DEG C ~ 720 DEG C and is incubated 1 ~ 2h in resistance furnace;
Step 5, heat is tender straight
6 rollers or the thick straightener of 10 rollers is used to carry out hot straightening and air cooling after the titanium alloy rod bar temperature of annealed process is down to 450 DEG C ~ 500 DEG C, then with Centreless lathe turning to finished product bar size (comprising surplus 1mm), put into 10 roller essence straighteners be heated to 400 DEG C ~ 450 DEG C again in chamber type electric resistance furnace after to align, reach the linearity of 0.5/1000mm, with not being in the mood for car or centreless grinding is processed into finished product bar size after flaw detection;
Step 6, finishing process
Put into 10 roller essence straighteners after the titanium alloy rod bar processed through step 5 being heated in chamber type electric resistance furnace 400 DEG C ~ 450 DEG C to align, reach the linearity of 0.5/1000mm, finally carry out twice polished finish, namely obtain Titanium Alloys for Surgical Implants bar.
Feature of the present invention is also,
The titanium alloy ingot selected in step 1, composed of the following components according to mass percent: Al5.5-6.5%, V3.5-4.5%, Fe≤0.2%, C≤0.08%, N≤0.03%, H≤0.006%, O≤0.13%, surplus is Ti, and said components mass percent sum is 100%.
In step 2, heating and thermal insulation carries out in resistance furnace, and Heating temperature is 1000 DEG C ~ 1150 DEG C, and soaking time is 3 ~ 5h.
In step 5, flaw detection titanium alloy rod bar is put into tank defect-detecting equipment to do ultrasonic testing.
The invention has the beneficial effects as follows, the preparation method of Titanium Alloys for Surgical Implants bar of the present invention, through three tender straight, three anneal, improve the quality and performance of titanium alloy rod bar, meet export requirement, the present invention makes its deformation rate reach 50 ~ 60% by after titanium alloy ingot heating and thermal insulation with hammering equipment in addition, then carry out pier and pull out 6 ~ 9 times, improve the degree of compactness of titanium alloy, and the temperature adopted in centre forging and mill product all lower than titanium alloy transformation temperature 970 DEG C thus ensure that performance and the metallographic structure of titanium alloy rod bar.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The preparation method of Titanium Alloys for Surgical Implants bar of the present invention, specifically implements according to following steps:
Step 1, blank prepares
Select the titanium alloy ingot meeting GB/T13810-2007 standard-required as blank, the titanium alloy ingot selected, composed of the following components according to mass percent: Al5.5 ~ 6.5%, V3.5 ~ 4.5%, Fe≤0.2%, C≤0.08%, N≤0.03%, H≤0.006%, O≤0.13%, surplus is Ti, and said components mass percent sum is 100%; The part of existing defects is determined in excision after UT (Ultrasonic Testing), is then divided into lathe chamfering on segment;
Step 2, cogging is forged
Titanium alloy ingot be heated in resistance furnace 1000 DEG C ~ 1150 DEG C and make its deformation rate reach 50 ~ 60% with hammering equipment after being incubated 3 ~ 5h, then carrying out being cut into finished product bar after pier pulls out 6 ~ 9 times needs the little titanium alloy briquet of weight;
Step 3, deformation processing
Little titanium alloy briquet step 2 obtained is heated to 930 DEG C ~ 960 DEG C after carrying out reconditioning (crackle and defect are fallen in reconditioning) and is incubated 1.5 ~ 2h in resistance furnace, then reconditioning again after ф 50 ~ ф 60 pole is broken into 1 ton of air hammer, in resistance furnace, be heated to 930 DEG C ~ 960 DEG C again and roll equipment with wire rod after being incubated 1 ~ 1.5h make its deformation rate reach 50% ~ 60%, make titanium alloy rod bar;
Step 4, anneal
Titanium alloy rod bar step 3 made is heated to 680 DEG C ~ 720 DEG C and is incubated 1 ~ 2h in resistance furnace;
Step 5, heat is tender straight
6 rollers or the thick straightener of 10 rollers is used to carry out hot straightening and air cooling after the titanium alloy rod bar temperature of annealed process is down to 450 DEG C ~ 500 DEG C, then with Centreless lathe turning to finished product bar size (comprising surplus 1mm), put into 10 roller essence straighteners be heated to 400 DEG C ~ 450 DEG C again in chamber type electric resistance furnace after to align, reach the linearity of 0.5/1000mm, with not being in the mood for car or centreless grinding is processed into finished product bar size after flaw detection; Flaw detection titanium alloy rod bar is put into tank defect-detecting equipment to do ultrasonic testing;
Step 6, finishing process
Put into 10 roller essence straighteners after the titanium alloy rod bar processed through step 5 being heated in chamber type electric resistance furnace 400 DEG C ~ 450 DEG C to align, reach the linearity of 0.5/1000mm, finally carry out twice polished finish, namely obtain Titanium Alloys for Surgical Implants bar.
The preparation method of Titanium Alloys for Surgical Implants bar of the present invention, tender straight through three times, three anneal, improve the quality and performance of titanium alloy rod bar, mechanical property after tested, tensile strength >=895MPa, yield strength >=828MPa, elongation after fracture >=10%, relative reduction in area >=25%, meet export requirement, the present invention makes its deformation rate reach 50 ~ 60% by after titanium alloy ingot heating and thermal insulation with hammering equipment in addition, then Dun order is carried out 6 ~ 9 times, improve the degree of compactness of titanium alloy, and in centre forging and mill product the temperature that adopts all lower than titanium alloy transformation temperature 970 DEG C thus ensure that performance and the metallographic structure of titanium alloy rod bar.
Embodiment 1
Step 1, blank prepares
Select the titanium alloy ingot meeting GB/T13810-2007 standard-required as blank, the titanium alloy ingot selected, composed of the following components according to mass percent: Al5.5%, V4.0%, Fe0.1%, C0.08%, N0.01%, H0.006%, O0.10%, surplus is Ti, and said components mass percent sum is 100%; The part of existing defects is determined in excision after UT (Ultrasonic Testing), is then divided into lathe chamfering on segment;
Step 2, cogging is forged
Titanium alloy ingot be heated in resistance furnace 1100 DEG C and make its deformation rate reach 50% with hammering equipment after being incubated 4h, then carrying out being cut into finished product bar after pier pulls out 6 times needs the little titanium alloy briquet of weight;
Step 3, deformation processing
Little titanium alloy briquet step 2 obtained is heated to 930 DEG C after carrying out reconditioning (crackle and defect are fallen in reconditioning) and is incubated 2h in resistance furnace, then reconditioning again after ф 50 pole is broken into 1 ton of air hammer, in resistance furnace, be heated to 930 DEG C again and roll equipment with wire rod after being incubated 1.5h make its deformation rate reach 60%, make titanium alloy rod bar;
Step 4, anneal
Titanium alloy rod bar step 3 made is heated to 700 DEG C and is incubated 1.8h in resistance furnace;
Step 5, heat is tender straight
The thick straightener of 6 roller is used to carry out hot straightening and air cooling after the titanium alloy rod bar temperature of annealed process is down to 480 DEG C, then with Centreless lathe turning to finished product bar size (comprising surplus 1mm), put into 10 roller essence straighteners after being heated to 400 DEG C again in chamber type electric resistance furnace to align, reach the linearity of 0.5/1000mm, with not being in the mood for car or centreless grinding is processed into finished product bar size after flaw detection; Flaw detection titanium alloy rod bar is put into tank defect-detecting equipment to do ultrasonic testing;
Step 6, finishing process
Put into 10 roller essence straighteners after the titanium alloy rod bar processed through step 5 is heated to 420 DEG C in chamber type electric resistance furnace to align, reach the linearity of 0.5/1000mm, finally carry out twice polished finish, namely obtain Titanium Alloys for Surgical Implants bar.
Titanium Alloys for Surgical Implants bar embodiment 1 prepared finds at 200 times of lower basis of microscopic observation, its microstructure meets the A1 level of ETTC2, for alpha-beta two-phase region is processed to form the tissue of good disperse, without the netted α of continuous print on original β crystal boundary, without the sheet α of thick elongation.
Carry out mechanical test to the Titanium Alloys for Surgical Implants bar that embodiment 1 prepares, result shows, and at temperature is 20 DEG C, tensile strength is 950MPa, and yield strength is 910MPa, and elongation after fracture is 20.4%, and relative reduction in area is 47%.
Embodiment 2
Step 1, blank prepares
Select the titanium alloy ingot meeting GB/T13810-2007 standard-required as blank, the titanium alloy ingot selected, composed of the following components according to mass percent: Al5.8%, V3.5%, Fe0.15%, N0.02%, H0.004%, O0.13%, surplus is Ti, and said components mass percent sum is 100%; The part of existing defects is determined in excision after UT (Ultrasonic Testing), is then divided into lathe chamfering on segment;
Step 2, cogging is forged
Titanium alloy ingot be heated in resistance furnace 1000 DEG C and make its deformation rate reach 60% with hammering equipment after being incubated 5h, then carrying out being cut into finished product bar after pier pulls out 9 times needs the little titanium alloy briquet of weight;
Step 3, deformation processing
Little titanium alloy briquet step 2 obtained is heated to 950 DEG C after carrying out reconditioning (crackle and defect are fallen in reconditioning) and is incubated 1.8h in resistance furnace, then reconditioning again after ф 55 pole is broken into 1 ton of air hammer, in resistance furnace, be heated to 950 DEG C again and roll equipment with wire rod after being incubated 1.2h make its deformation rate reach 55%, make titanium alloy rod bar;
Step 4, anneal
Titanium alloy rod bar step 3 made is heated to 680 DEG C and is incubated 2h in resistance furnace;
Step 5, heat is tender straight
The thick straightener of 10 roller is used to carry out hot straightening and air cooling after the titanium alloy rod bar temperature of annealed process is down to 460 DEG C, then with Centreless lathe turning to finished product bar size (comprising surplus 1mm), put into 10 roller essence straighteners after being heated to 420 DEG C again in chamber type electric resistance furnace to align, reach the linearity of 0.5/1000mm, with not being in the mood for car or centreless grinding is processed into finished product bar size after flaw detection; Flaw detection titanium alloy rod bar is put into tank defect-detecting equipment to do ultrasonic testing;
Step 6, finishing process
Put into 10 roller essence straighteners after the titanium alloy rod bar processed through step 5 is heated to 450 DEG C in chamber type electric resistance furnace to align, reach the linearity of 0.5/1000mm, finally carry out twice polished finish, namely obtain Titanium Alloys for Surgical Implants bar.
Embodiment 3
Step 1, blank prepares
Select the titanium alloy ingot meeting GB/T13810-2007 standard-required as blank, the titanium alloy ingot selected, composed of the following components according to mass percent: Al6.0%, V4.5%, Fe0.2%, C0.05%, H0.003%, O0.05%, surplus is Ti, and said components mass percent sum is 100%; The part of existing defects is determined in excision after UT (Ultrasonic Testing), is then divided into lathe chamfering on segment;
Step 2, cogging is forged
Titanium alloy ingot be heated in resistance furnace 1150 DEG C and make its deformation rate reach 55% with hammering equipment after being incubated 3h, then carrying out being cut into finished product bar after pier pulls out 8 times needs the little titanium alloy briquet of weight;
Step 3, deformation processing
Little titanium alloy briquet step 2 obtained is heated to 960 DEG C after carrying out reconditioning (crackle and defect are fallen in reconditioning) and is incubated 1.5h in resistance furnace, then reconditioning again after ф 60 pole is broken into 1 ton of air hammer, in resistance furnace, be heated to 960 DEG C again and roll equipment with wire rod after being incubated 1h make its deformation rate reach 55%, make titanium alloy rod bar;
Step 4, anneal
Titanium alloy rod bar step 3 made is heated to 720 DEG C and is incubated 1h in resistance furnace;
Step 5, heat is tender straight
The thick straightener of 10 roller is used to carry out hot straightening and air cooling after the titanium alloy rod bar temperature of annealed process is down to 450 DEG C, then with Centreless lathe turning to finished product bar size (comprising surplus 1mm), put into 10 roller essence straighteners after being heated to 450 DEG C again in chamber type electric resistance furnace to align, reach the linearity of 0.5/1000mm, with not being in the mood for car or centreless grinding is processed into finished product bar size after flaw detection; Flaw detection titanium alloy rod bar is put into tank defect-detecting equipment to do ultrasonic testing;
Step 6, finishing process
Put into 10 roller essence straighteners after the titanium alloy rod bar processed through step 5 is heated to 410 DEG C in chamber type electric resistance furnace to align, reach the linearity of 0.5/1000mm, finally carry out twice polished finish, namely obtain Titanium Alloys for Surgical Implants bar.
Embodiment 4
Step 1, blank prepares
Select the titanium alloy ingot meeting GB/T13810-2007 standard-required as blank, the titanium alloy ingot selected, composed of the following components according to mass percent: Al6.5%, V4.2%, C0.02%, N0.03%, H0.001%, O0.08%, surplus is Ti, and said components mass percent sum is 100%; The part of existing defects is determined in excision after UT (Ultrasonic Testing), is then divided into lathe chamfering on segment;
Step 2, cogging is forged
Titanium alloy ingot be heated in resistance furnace 1050 DEG C and make its deformation rate reach 55% with hammering equipment after being incubated 3.5h, then carrying out being cut into finished product bar after pier pulls out 7 times needs the little titanium alloy briquet of weight;
Step 3, deformation processing
Little titanium alloy briquet step 2 obtained is heated to 940 DEG C after carrying out reconditioning (crackle and defect are fallen in reconditioning) and is incubated 1.6h in resistance furnace, then reconditioning again after ф 60 pole is broken into 1 ton of air hammer, in resistance furnace, be heated to 940 DEG C again and roll equipment with wire rod after being incubated 1.2h make its deformation rate reach 50%, make titanium alloy rod bar;
Step 4, anneal
Titanium alloy rod bar step 3 made is heated to 690 DEG C and is incubated 1.5h in resistance furnace;
Step 5, heat is tender straight
The thick straightener of 6 roller is used to carry out hot straightening and air cooling after the titanium alloy rod bar temperature of annealed process is down to 500 DEG C, then with Centreless lathe turning to finished product bar size (comprising surplus 1mm), put into 10 roller essence straighteners after being heated to 430 DEG C again in chamber type electric resistance furnace to align, reach the linearity of 0.5/1000mm, with not being in the mood for car or centreless grinding is processed into finished product bar size after flaw detection; Flaw detection titanium alloy rod bar is put into tank defect-detecting equipment to do ultrasonic testing;
Step 6, finishing process
Put into 10 roller essence straighteners after the titanium alloy rod bar processed through step 5 is heated to 400 DEG C in chamber type electric resistance furnace to align, reach the linearity of 0.5/1000mm, finally carry out twice polished finish, namely obtain Titanium Alloys for Surgical Implants bar.
Claims (4)
1. the preparation method of Titanium Alloys for Surgical Implants bar, is characterized in that, specifically implements according to following steps:
Step 1, blank prepares
Select the titanium alloy ingot meeting GB/T 13810-2007 standard-required as blank, excise the part determining existing defects after UT (Ultrasonic Testing), be then divided into lathe chamfering on segment;
Step 2, cogging is forged
Make its deformation rate reach 50 ~ 60% by after titanium alloy ingot heating and thermal insulation with hammering equipment, then carrying out being cut into finished product bar after pier pulls out 6 ~ 9 times needs the little titanium alloy briquet of weight;
Step 3, deformation processing
Little titanium alloy briquet step 2 obtained carries out reconditioning, crackle and defect are fallen in reconditioning, then in resistance furnace, be heated to 930 DEG C ~ 960 DEG C and be incubated 1.5 ~ 2h, then reconditioning again after ф 50 ~ ф 60 pole is broken into 1 ton of air hammer, in resistance furnace, be heated to 930 DEG C ~ 960 DEG C again and make its deformation rate reach 50% ~ 60% with rod rolling equipment after being incubated 1 ~ 1.5h, making titanium alloy rod bar;
Step 4, anneal
Titanium alloy rod bar step 3 made is heated to 680 DEG C ~ 720 DEG C and is incubated 1 ~ 2h in resistance furnace;
Step 5, hot straightening
6 rollers or the thick straightener of 10 rollers is used to carry out hot straightening and air cooling after the titanium alloy rod bar temperature of annealed process is down to 450 DEG C ~ 500 DEG C, then use Centreless lathe turning to finished product bar size, comprise surplus 1mm, put into 10 roller essence straighteners be heated to 400 DEG C ~ 450 DEG C again in chamber type electric resistance furnace after to align, reach the linearity of 0.5/1000mm, with not being in the mood for car or centreless grinding is processed into finished product bar size after flaw detection;
Step 6, finishing process
Put into 10 roller essence straighteners after the titanium alloy rod bar processed through step 5 being heated in chamber type electric resistance furnace 400 DEG C ~ 450 DEG C to align, reach the linearity of 0.5/1000mm, finally carry out twice polished finish, namely obtain Titanium Alloys for Surgical Implants bar.
2. the preparation method of Titanium Alloys for Surgical Implants bar according to claim 1, it is characterized in that, the titanium alloy ingot selected in described step 1, composed of the following components according to mass percent: Al5.5-6.5%, V 3.5-4.5%, Fe≤0.2%, C≤0.08%, N≤0.03%, H≤0.006%, O≤0.13%, surplus is Ti, and said components mass percent sum is 100%.
3. the preparation method of Titanium Alloys for Surgical Implants bar according to claim 1, is characterized in that, in described step 2, heating and thermal insulation carries out in resistance furnace, and Heating temperature is 1000 DEG C ~ 1150 DEG C, and soaking time is 3 ~ 5h.
4. the preparation method of Titanium Alloys for Surgical Implants bar according to claim 1, is characterized in that, in described step 5, flaw detection titanium alloy rod bar is put into tank defect-detecting equipment to do ultrasonic testing.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104962779A (en) * | 2015-07-31 | 2015-10-07 | 创生医疗器械（中国）有限公司 | Ti6Al4V alloy and orthopaedic implant prepared from alloy |
| US10851437B2 (en) * | 2016-05-18 | 2020-12-01 | Carpenter Technology Corporation | Custom titanium alloy for 3-D printing and method of making same |
| CN106180251B (en) * | 2016-08-16 | 2018-05-08 | 西部超导材料科技股份有限公司 | A kind of preparation method of TC20 titanium alloys fine grain bar |
| CN106826118B (en) * | 2017-02-08 | 2018-09-14 | 大连盛辉钛业有限公司 | A kind of preparation method for manufacturing the medical titanium alloy bar of pedicle screw |
| CN107138523B (en) * | 2017-06-29 | 2019-07-02 | 西部超导材料科技股份有限公司 | A kind of TB9 titanium alloy wire bar and its milling method |
| CN107443028A (en) * | 2017-09-25 | 2017-12-08 | 宝鸡市永盛泰钛业有限公司 | A kind of preparation method of high strength titanium alloy bar |
| CN110369655B (en) * | 2019-08-08 | 2020-08-21 | 无锡航亚科技股份有限公司 | Forging method of CoCrMo tibial plateau artificial joint implant |
| CN111286686B (en) * | 2020-04-09 | 2021-09-10 | 西部钛业有限责任公司 | Short-process preparation method of TC4 titanium alloy large-size bar with fine equiaxial structure |
| CN111545995A (en) * | 2020-04-22 | 2020-08-18 | 西安圣泰金属材料有限公司 | Titanium alloy bar for minimally invasive pedicle screw and preparation method thereof |
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| CN102230097A (en) * | 2011-03-31 | 2011-11-02 | 西北有色金属研究院 | Preparation method of titanium alloy bars |
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