CN105598199B - A kind of preparation method of titanium fiber - Google Patents
A kind of preparation method of titanium fiber Download PDFInfo
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- CN105598199B CN105598199B CN201510765620.9A CN201510765620A CN105598199B CN 105598199 B CN105598199 B CN 105598199B CN 201510765620 A CN201510765620 A CN 201510765620A CN 105598199 B CN105598199 B CN 105598199B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
- B21C37/042—Manufacture of coated wire or bars
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
- B21C37/047—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire of fine wires
Abstract
The invention discloses a kind of preparation method of titanium fiber, titanium silk through overpickling, nickel preplating, copper coating, obtains copper facing titanium silk successively；Copper facing titanium silk is dried, vacuum annealing process after boundling is compound, then bundle drawing method is handled, and obtains complex；Complex is washed after overpickling, drying.The preparation method of titanium fiber of the present invention, it instead of monofilament drawing in the production of titanium fiber, greatly increase the production efficiency, reduce production cost, it ensure that batch production titanium fibre property stability, improve product quality, it is most important that solve the problems, such as that a diameter of below 0.1mm titaniums silk is difficult to, prepared multicore, the titanium fiber of 25 μm of minimum diameter.
Description
Technical field
The invention belongs to metal working technical area, and in particular to a kind of preparation method of titanium fiber.
Background technology
Titanium fiber have density is small, intensity is high, high temperature resistant, excellent comprehensive mechanical property and the excellent biology such as corrosion-resistant
Compatibility and other unique properties, show according to related document, titanium silk (especially a diameter of below 0.1mm) and implantation material heterozygosis
After change, the high-affinity of cell can be also improved, and then improve the combination of bone and implant.Just because of so many excellent of titanium alloy
Point, has become one of popular high end materials that the fields such as bio-medical, Aeronautics and Astronautics, ocean, military project, physical culture use at present.Mesh
It is preceding to be widely used in the high-tech areas such as medical operation suture thread, water treatment system, intelligence sensor and suit, still
Since the production of titanium silk is easily damaged using the processing method of monofilament multi-pass, small compression ratio silk, mould mostly, easy fracture of wire, is caused
Production cost is quite high, and the finished surface quality index of production is extremely difficult to medical grade requirement, and the credit rating of product is widely different,
And the minimum only Φ 0.1mm of pure titanium silk material specification produced at present, limit application of the titanium fiber in high-end field.
At present, there are no the report (a diameter of below 0.1mm) of titanium fiber, existing associated fiber silk be all stainless steel and
Other metals, have no the filametntary patent of titanium.
The content of the invention
The object of the present invention is to provide a kind of preparation method of titanium fiber, solves the silk material minimum silk that existing method obtains
Through there was only Φ 0.1mm, the problem of titanium fiber is applied in high-end field is limited.
The technical solution adopted in the present invention is that a kind of preparation method of titanium fiber, specifically implements according to following steps：
Step 1, titanium silk obtains copper facing titanium silk successively through overpickling, nickel preplating, copper coating；
Step 2, copper facing titanium silk step 1 obtained is dried, vacuum annealing process after boundling is compound, then at bundle drawing method
Reason, obtains complex；
Step 3, complex step 2 obtained is washed after overpickling, and drying, obtains titanium fiber.
The features of the present invention also resides in,
In step 1 using automatic coil winding machine make a diameter of 0.4~0.6mm titaniums silk successively by descaling bath and nickel preplating groove into
Row activation process and plating nickel on surface, finally enter main coating bath and obtain copper facing titanium silk, wherein closely coupled between each groove；Automatically around
Line machine speed is 60~200r/min.
Pickle is composed of the following components by mass percentage in descaling bath：Nitric acid 15~25%, hydrofluoric acid 3~5% are remaining
It is 100% to measure as the sum of water, said components mass percent, and pickling time is 20~30s.
The mass concentration of nitric acid is 65%, and the mass concentration of hydrofluoric acid is 40%.
The component of plating solution is in nickel preplating groove：100~150g/L of nickel chloride, 150~250ml/L's of hydrochloric acid, wherein hydrochloric acid
Mass concentration is 34%, and preplating current density is 4~10A/dm2, the time is 3~5min.
The component of plating solution is in main coating bath：25~50ml/L of the concentrated sulfuric acid, 100~300g/L of cupric sulfate pentahydrate, main plating electric current
Density is 0.5~5A/mm2, temperature is 15~40 DEG C, and the time is 25~30min.
The temperature of vacuum annealing process is 600~660 DEG C in step 2, and vacuum is not more than 10-3Pa, the time for 0.1~
1h。
It is 5~15% to control pass reduction in step 2 in bundle drawing method processing procedure, and total deformation is 60~70%；
In drawing process to complex carry out middle vacuum annealing, control first time intermediate annealing total deformation be 60~
70%, the total deformation between adjacent intermediate annealing twice is 60~70%, and annealing temperature and soaking time are gradually reduced to subtract
Little crystal grain is grown up and thickness of diffusion layer, the silk material surface coating lubricant in drawing process.
The pickle that pickling uses in step 3 is combined to obtain by water, nitric acid and hydrochloric acid, wherein the body of water, hydrochloric acid and nitric acid
Product is than being 4~7：2~5：1, the mass concentration of nitric acid and hydrochloric acid is respectively 20~65% and 25~30%.
The invention has the advantages that the preparation method of titanium fiber of the present invention, monofilament is instead of in the production of titanium fiber
Drawing, greatly increases the production efficiency, and reduces production cost, ensure that batch production titanium fibre property stability, improves
Product quality, it is most important that solve the problems, such as that a diameter of below 0.1mm titaniums silk is difficult to, prepared multicore, minimum
The titanium fiber of 25 μm of diameter.
Brief description of the drawings
Fig. 1 is the cross-sectional scans figure for the titanium fiber composite that the present invention is prepared.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The preparation method of titanium fiber of the present invention, specifically implements according to following steps：
Step 1, speed is used a diameter of 0.4~0.6mm titaniums silk is passed through successively for 60~200r/min automatic coil winding machines
Descaling bath and nickel preplating groove carry out activation process and plating nickel on surface, finally enter main coating bath and obtain copper facing titanium silk, wherein each groove
Between it is closely coupled, to prevent that titanium silk is long and generate oxide-film again on surface exposed to air time；
Pickle is composed of the following components by mass percentage in descaling bath：Nitric acid (mass concentration 65%) 15~
25%, hydrofluoric acid (mass concentration 40%) 3~5%, surplus is that the sum of water, said components mass percent is 100%, pickling
Time is 20~30s；
The component of plating solution is in nickel preplating groove：100~150g/L of nickel chloride, hydrochloric acid (mass concentration 34%) 150~
The mass concentration of 250ml/L, wherein hydrochloric acid are 34%, and preplating current density is 4~10A/dm2, the time is 3~5min；
The component of plating solution is in main coating bath：25~50ml/L of the concentrated sulfuric acid, 100~300g/L of cupric sulfate pentahydrate, main plating electric current
Density is 0.5~5A/mm2, temperature is 15~40 DEG C, and the time is 20~30min.
Step 2, copper facing titanium silk step 1 obtained is dried, vacuum annealing process after boundling is compound, and temperature is 600~650
DEG C, vacuum is not more than 10-3Pa, time are 0.3~1h, and then bundle drawing method is handled, and obtains complex；Bundle drawing method treats
It is 5~15% that pass reduction is controlled in journey, and total deformation is 60~70%；Middle vacuum is carried out to complex in drawing process
Annealing, the total deformation for controlling first time intermediate annealing are 60~70%, the total deformation between adjacent intermediate annealing twice
Measure as 60~70%, annealing temperature and soaking time are gradually reduced is grown up and thickness of diffusion layer with reducing crystal grain, in drawing process
In silk material surface coating lubricant；
Drawing after the secondary boundling tubulature of complex will can also be made annealing treatment according to actual needs, obtains secondary multiple
It is fit.
Step 3, by the complex that step 2 obtains through overpickling, pickle is by water, hydrochloric acid and nitric acid (mass concentration 20
~30%) combination obtains, and wherein the volume ratio of water, hydrochloric acid and nitric acid is 4~7：2~5：1；It is clear by multiple deionized water again
Wash, finally obtain titanium fiber after 40~60 DEG C of drying.
The effect of pickling is to remove surface layers of copper in step 3, while can also erode the titanium copper diffusion layer that annealing produces.
The preparation method of titanium fiber of the present invention, by copper coating again after pickling and nickel preplating processing, overcomes titanium silk
The problem of overlay coating combination force difference；Titanium copper composite pipe is processed into by complex using drawing tube reducing technology, passes through technological parameter
Stringent control overcome the problems such as titanium is oxidizable, processing hardening is serious；The corrosion of mixed acid solution is finally carried out to complex,
Overlay coating and diffusion layer successfully are eliminated, prepares Multi-core number, the titanium fiber that minimum diameter is 25 μm.
The section of the titanium fiber composite that the present invention is prepared is as shown in Figure 1, present invention side it can be seen from Fig. 1
Method causes adjacent titanium silk to separate, and ensure that will not stick together between titanium silk during bundle drawing method, titanium fiber surface shape
State is good.
Embodiment 1
Step 1, silk is passed through to pure titanium (TA1) the alcohol wipe grease removal for being 0.4mm first, then is cleaned and done with deionized water
Only, speed is used titanium silk is carried out activation process and table by descaling bath and nickel preplating groove successively for 60r/min automatic coil winding machines
Face nickel plating, finally enters main coating bath and obtains copper facing titanium silk；
Pickle is composed of the following components by mass percentage in descaling bath：Nitric acid (mass concentration 65%) 18%, hydrogen
Fluoric acid (mass concentration 40%) 3%, surplus are that the sum of water, said components mass percent is 100%, pickling time 30s；
The component of plating solution is in nickel preplating groove：Nickel chloride 120g/L, hydrochloric acid (mass concentration 34%) 160ml/L, wherein
The mass concentration of hydrochloric acid is 34%, and preplating current density is 5A/dm2, time 3min；
The component of plating solution is in main coating bath：Concentrated sulfuric acid 30ml/L, cupric sulfate pentahydrate 140g/L, main plating current density is 3A/
mm2, temperature is 25 DEG C, time 20min.
Step 2, after copper facing titanium silk drying step 1 obtained after the copper tube of 12 × 2mm of boundling loading Φ on broaching machine
Compound, it is 200 to obtain core number, and a diameter of 8.1 multiple tube, is then placed into vacuum annealing furnace by multiple tube and carries out at annealing
Reason, annealing temperature are 640 DEG C, soaking time 50min, and vacuum is 6 × 10-2Pa, air quenching is carried out after reaching soaking time immediately
Processing, then the complex after annealing is subjected to drawing, annealing temperature selection is drawn to Φ 5.0, Φ in complex diameter
3.0th, anneal when Φ 1.7, Φ 1, Φ 0.7, annealing temperature and soaking time gradually reduce and grow up and spread to reduce crystal grain
Layer thickness, design parameter is 630 DEG C × 40min, 620 DEG C × 30min, 610 DEG C × 20min, 600 DEG C × 10min, and vacuum is not
More than 5 × 10-2Pa, finally obtains the composite filament that string diameter is 0.5mm.
Step 3, by the complex that step 2 obtains through overpickling, pickle is by water, hydrochloric acid and nitric acid (mass concentration 20
~30%) combination obtains, and wherein salpeter solution concentration is 20ml/L, concentration of hydrochloric acid solution 50ml/L；Again by repeatedly go from
Sub- water cleaning, finally obtains 200 cores, the titanium fiber that string diameter is 30 μm after 40 DEG C of drying.
Embodiment 2
Step 1, silk is passed through to pure titanium (TA1) the alcohol wipe grease removal for being 0.5mm first, then is cleaned and done with deionized water
Only, speed is used titanium silk is carried out activation process and table by descaling bath and nickel preplating groove successively for 120r/min automatic coil winding machines
Face nickel plating, finally enters main coating bath and obtains copper facing titanium silk；
Pickle is composed of the following components by mass percentage in descaling bath：Nitric acid (mass concentration 65%) 21%, hydrogen
Fluoric acid (mass concentration 40%) 4%, surplus are that the sum of water, said components mass percent is 100%, pickling time 25s；
The component of plating solution is in nickel preplating groove：Nickel chloride 130g/L, hydrochloric acid (mass concentration 34%) 200ml/L, wherein
The mass concentration of hydrochloric acid is 34%, and preplating current density is 7A/dm2, time 4min；
The component of plating solution is in main coating bath：Concentrated sulfuric acid 40ml/L, cupric sulfate pentahydrate 200g/L, main plating current density is 4A/
mm2, temperature is 28 DEG C, time 25min.
Step 2, after copper facing titanium silk drying step 1 obtained after the copper tube of 14 × 2mm of boundling loading Φ on broaching machine
Compound, it is 250 to obtain core number, and a diameter of 9.2 multiple tube, is then placed into vacuum annealing furnace by multiple tube and carries out at annealing
Reason, annealing temperature are 650 DEG C, soaking time 1h, and vacuum is 5 × 10-2Pa, carries out at air quenching immediately after reaching soaking time
Reason, then by after annealing complex carry out drawing, annealing temperature selection complex diameter be drawn to Φ 5.3, Φ 3.2,
Anneal when Φ 2.0, Φ 1.2, Φ 0.8, annealing temperature and soaking time are gradually reduced is grown up and diffusion layer with reducing crystal grain
Thickness, design parameter is 640 DEG C × 40min, 630 DEG C × 30min, 620 DEG C × 20min, 610 DEG C × 10min, and vacuum is little
In 5 × 10-2Pa, finally obtains the composite filament that string diameter is 0.5mm.
Step 3, by the complex that step 2 obtains through overpickling, pickle is by water, hydrochloric acid and nitric acid (mass concentration 20
~30%) combination obtains, and wherein salpeter solution concentration is 25ml/L, concentration of hydrochloric acid solution 60ml/L；Again by repeatedly go from
Sub- water cleaning, finally obtains 250 cores, the titanium fiber that string diameter is 27 μm after 50 DEG C of drying.
Embodiment 3
Step 1, silk is passed through to pure titanium (TA1) the alcohol wipe grease removal for being 0.6mm first, then is cleaned and done with deionized water
Only, speed is used titanium silk is carried out activation process and table by descaling bath and nickel preplating groove successively for 160r/min automatic coil winding machines
Face nickel plating, finally enters main coating bath and obtains copper facing titanium silk；
Pickle is composed of the following components by mass percentage in descaling bath：Nitric acid (mass concentration 65%) 24%, hydrogen
Fluoric acid (mass concentration 40%) 5%, surplus are that the sum of water, said components mass percent is 100%, pickling time 20s；
The component of plating solution is in nickel preplating groove：Nickel chloride 150g/L, hydrochloric acid (mass concentration 34%) 240ml/L, wherein
The mass concentration of hydrochloric acid is 34%, and preplating current density is 9A/dm2, time 5min；
The component of plating solution is in main coating bath：Concentrated sulfuric acid 50ml/L, cupric sulfate pentahydrate 250g/L, main plating current density is 5A/
mm2, temperature is 35 DEG C, time 30min.
Step 2, after copper facing titanium silk drying step 1 obtained after the copper tube of 16 × 2mm of boundling loading Φ on broaching machine
Compound, it is 300 to obtain core number, and a diameter of 10.1 multiple tube, is then placed into vacuum annealing furnace by multiple tube and carries out at annealing
Reason, annealing temperature are 650 DEG C, soaking time 1h, and vacuum is 4 × 10-2Pa, carries out at air quenching immediately after reaching soaking time
Reason, then by after annealing complex carry out drawing, annealing temperature selection complex diameter be drawn to Φ 5.8, Φ 3.5,
Anneal when Φ 2.2, Φ 1.3, Φ 0.8, annealing temperature and soaking time are gradually reduced is grown up and diffusion layer with reducing crystal grain
Thickness, design parameter is 650 DEG C × 50min, 640 DEG C × 40min, 630 DEG C × 30min, 620 DEG C × 20min, and vacuum is little
In 4 × 10-2Pa, finally obtains the composite filament that string diameter is 0.5mm.
Step 3, by the complex that step 2 obtains through overpickling, pickle is by water, hydrochloric acid and nitric acid (mass concentration 20
~30%) combination obtains, and wherein salpeter solution concentration is 25ml/L, concentration of hydrochloric acid solution 50ml/L；Again by repeatedly go from
Sub- water cleaning, finally obtains 300 cores, the titanium fiber that string diameter is 25 μm after 60 DEG C of drying.
Claims (4)
1. a kind of preparation method of titanium fiber, it is characterised in that specifically implement according to following steps：
Step 1, titanium silk obtains copper facing titanium silk successively through overpickling, nickel preplating, copper coating, is specially：Using automatic coil winding machine
A diameter of 0.4~0.6mm titaniums silk is carried out activation process and plating nickel on surface by descaling bath and nickel preplating groove successively, finally enter
Main coating bath obtains copper facing titanium silk, wherein closely coupled between each groove；Automatic coil winding machine speed is 60~200r/min, wherein,
Pickle is composed of the following components by mass percentage in descaling bath：Nitric acid 15~25%, hydrofluoric acid 3~5%, surplus are water,
The sum of said components mass percent is 100%, and pickling time is 20~30s, and the mass concentration of nitric acid is 65%, hydrofluoric acid
Mass concentration is 40%；
Step 2, copper facing titanium silk step 1 obtained is dried, vacuum annealing process after boundling is compound, the temperature of vacuum annealing process
For 600~660 DEG C, vacuum is not more than 10-3Pa, time are 0.1~1h, and air quenching processing is carried out immediately after reaching soaking time,
Then bundle drawing method is handled, and obtains complex, and it is 5~15% that pass reduction is controlled in bundle drawing method processing procedure, total deformation
Measure as 60~70%；Middle vacuum annealing, total change of control first time intermediate annealing are carried out in drawing process to complex
Shape amount is 60~70%, and total deformation between adjacent intermediate annealing twice is 60~70%, annealing temperature and soaking time by
Step is reduced is grown up and thickness of diffusion layer with reducing crystal grain, the silk material surface coating lubricant in drawing process；
Step 3, complex step 2 obtained is washed after overpickling, and drying, obtains titanium fiber.
A kind of 2. preparation method of titanium fiber according to claim 1, it is characterised in that the component of plating solution in nickel preplating groove
For：The mass concentration of 100~150g/L of nickel chloride, wherein 150~250ml/L of hydrochloric acid, hydrochloric acid are 34%, and preplating current density is
4~10A/dm2, the time is 3~5min.
A kind of 3. preparation method of titanium fiber according to claim 1, it is characterised in that the component of plating solution in main coating bath
For：25~50ml/L of the concentrated sulfuric acid, 100~300g/L of cupric sulfate pentahydrate, main plating current density is 0.5~5A/mm2, temperature 15
~40 DEG C, the time is 25~30min.
A kind of 4. preparation method of titanium fiber according to claim 1, it is characterised in that the acid that pickling uses in step 3
Washing lotion is combined to obtain by water, nitric acid and hydrochloric acid, and wherein the volume ratio of water, hydrochloric acid and nitric acid is 4~7：2~5：1, nitric acid and hydrochloric acid
Mass concentration be respectively 20~65% and 25~30%.
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| CN111715722B (en) * | 2020-06-19 | 2022-05-27 | 西安菲尔特金属过滤材料股份有限公司 | Preparation method of multi-core-number blended metal fiber for X and gamma ray protection |
| CN112246894B (en) * | 2020-09-28 | 2023-08-18 | 湖南汇博金属材料有限责任公司 | Production process of titanium fiber |
| CN114713658B (en) * | 2022-04-21 | 2023-09-22 | 湖南惠同新材料股份有限公司 | Manufacturing method of titanium fiber |
| CN114535343B (en) * | 2022-04-26 | 2022-08-30 | 西部宝德科技股份有限公司 | Titanium fiber preparation method |
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| JPH1181050A (en) * | 1997-09-01 | 1999-03-26 | Bridgestone Metalpha Kk | Titanium fiber and its production |
| JP2001025813A (en) * | 1999-07-13 | 2001-01-30 | Bridgestone Corp | Manufacture of titanium fiber or titanium alloy fiber |
| JP5268183B2 (en) * | 2007-06-11 | 2013-08-21 | 株式会社ハイレックスコーポレーション | Titanium long fiber and method for producing the same |
| CN103233254B (en) * | 2013-04-11 | 2015-05-13 | 西安菲尔特金属过滤材料有限公司 | Preparation method of corrosion resistant alloy fiber |
| CN103611757B (en) * | 2013-12-10 | 2015-08-19 | 西部新锆核材料科技有限公司 | A kind of preparation method of zirconium metal fiber wire |
| CN104928739B (en) * | 2015-06-30 | 2018-05-01 | 西安菲尔特金属过滤材料有限公司 | A kind of wire rod continuous electric plating device and method |
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Address after: 710201 Shaanxi city of Xi'an Province Economic and Technological Development Zone Jingwei Industrial Park Road No. 15 Patentee after: Xi'an ferro metal filter material Co.,Ltd. Address before: 710201 Shaanxi city of Xi'an Province Economic and Technological Development Zone Jingwei Industrial Park Road No. 15 Patentee before: XI'AN FILTER METAL MATERIALS Co.,Ltd. |