CN117144166A - Production method and production device of medical nickel-titanium alloy wire - Google Patents
Production method and production device of medical nickel-titanium alloy wire Download PDFInfo
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- CN117144166A CN117144166A CN202311096003.5A CN202311096003A CN117144166A CN 117144166 A CN117144166 A CN 117144166A CN 202311096003 A CN202311096003 A CN 202311096003A CN 117144166 A CN117144166 A CN 117144166A
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- 229910001000 nickel titanium Inorganic materials 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 70
- 238000003723 Smelting Methods 0.000 claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 44
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000010936 titanium Substances 0.000 claims abstract description 35
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 34
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 238000005491 wire drawing Methods 0.000 claims abstract description 23
- 238000012545 processing Methods 0.000 claims abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 238000004381 surface treatment Methods 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims description 28
- 230000008018 melting Effects 0.000 claims description 28
- 238000001816 cooling Methods 0.000 claims description 25
- 238000005242 forging Methods 0.000 claims description 20
- 238000005098 hot rolling Methods 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 10
- 230000006698 induction Effects 0.000 claims description 10
- 238000007670 refining Methods 0.000 claims description 9
- 238000009826 distribution Methods 0.000 claims description 8
- 238000010894 electron beam technology Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 6
- 238000005096 rolling process Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 238000010622 cold drawing Methods 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 description 9
- 239000012535 impurity Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000005484 gravity Effects 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 5
- 229910001285 shape-memory alloy Inorganic materials 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- MOWMLACGTDMJRV-UHFFFAOYSA-N nickel tungsten Chemical compound [Ni].[W] MOWMLACGTDMJRV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000002792 vascular Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/04—Non-resorbable materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/02—Inorganic materials
- A61L31/022—Metals or alloys
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Vascular Medicine (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Surgery (AREA)
- Physics & Mathematics (AREA)
- Heart & Thoracic Surgery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a production method of a medical nickel-titanium alloy wire, which comprises the following steps of; (1) Carrying out vacuum suspension smelting and vacuum consumable arc smelting on the purified nickel material and titanium material to obtain an ingot; (2) And (3) sequentially carrying out a thermal processing technology, wire drawing and surface treatment on the cast ingot to obtain the medical nickel-titanium alloy wire. The invention starts from the basic process of nickel-titanium alloy wire production, comprehensively improves the existing process method in the aspects of component precise control technology, ingot smelting process method, hot working process, heat treatment process and tissue property adjustment control, improves the uniformity, stability and consistency of nickel-titanium alloy wire products, and lays a good foundation for the production of high-level medical devices.
Description
Technical Field
The invention relates to the technical field of alloy wire processing, in particular to a production method and a production device of a medical nickel-titanium alloy wire.
Background
Nickel-titanium alloy is one of the metallic materials frequently used in clinical medicine, and is also called "nickel-titanium memory alloy" because it has a temperature shape memory effect. On one hand, according to the different proportions of nickel and titanium in the alloy, the phase change points are different, so that the memory original device at different temperatures can be manufactured; on the other hand, nickel-titanium alloys have excellent superelasticity and biocompatibility, which are far higher than other metal alloys, and thus are increasingly used in medical treatment. Therefore, the medical device is mainly applied to medical devices such as a vascular stent, an anastomotic line in an anastomat, oral cavity tooth orthotics, ultrasonic knife manufacturing and the like at present.
The nickel-titanium alloy is mainly processed by wires and plates, and is a high-end medical material which is true because of high component sensitivity, narrow hot processing temperature range, high cold processing resistance and high manufacturing difficulty.
Therefore, the nickel-titanium alloy wire with uniform material composition and stable performance and the production method thereof are problems to be solved by the technicians in the field.
Disclosure of Invention
The invention aims to provide a production method and a production device of a medical nickel-titanium alloy wire.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the production process of medical nickel-titanium alloy wire includes the following steps;
(1) Carrying out vacuum suspension smelting and vacuum consumable arc smelting on the purified nickel material and titanium material to obtain an ingot;
(2) And (3) sequentially carrying out a thermal processing technology, wire drawing and surface treatment on the cast ingot to obtain the medical nickel-titanium alloy wire.
The nickel-titanium alloy is particularly sensitive to components, the performance is greatly reduced due to pollution in the process of smelting and casting ingots, and the crucible pollution cannot be prevented at all when a plurality of manufacturing enterprises use alkaline crucibles such as ceramics for vacuum induction smelting the nickel-titanium alloy, because molten titanium is very movable at high temperature and can react with any oxynitride, and the nickel-titanium alloy is one of the reasons of poor quality. Because the cooling speed of the cast ingot cannot be controlled in the simple vacuum induction furnace smelting, coarse tissues with different degrees can be caused, and the subsequent hot processing performance can be seriously affected, so that the invention adopts a brand-new duplex smelting technology: the combination melting of vacuum suspension melting and vacuum consumable arc melting ensures the uniformity of components and no crucible material pollution by induction melting on one hand, and ensures the consistency of ingot tissue by consumable remelting on the other hand.
Preferably, the purity of the nickel and titanium materials in the step (1) is 4N5;
the purification method is characterized in that the nickel material and the titanium material are respectively smelted and purified by adopting vacuum electron beams, and the specific steps are as follows:
nickel material: repeatedly melting, cooling and refining the nickel material for at least three times at 1400-2450 ℃;
titanium material: and (3) repeatedly melting, cooling and refining the titanium material for at least three times at 1600-2800 ℃.
The memory alloy adopted by the invention is nickel-titanium binary alloy, the purity of nickel and titanium has a decisive influence on the performance of the memory alloy, and the highest-grade purity of electrolytic nickel and sponge titanium only can reach the level of about 2N5 (99.5 percent), so that the use requirement of the memory alloy cannot be met at all, which is an important reason that the performance of the produced memory alloy is always unstable; the principle of the method is that the ultra-high temperature (more than 2800 ℃) generated by electron beams is utilized to smelt the nickel and the titanium respectively, and the different solubility and evaporation speed of non-metallic impurities such as oxygen, nitrogen, carbon, sulfur and the like under high vacuum state are utilized to continuously reduce the content of the non-metallic impurities in molten metal so as to achieve the aim of purification.
Preferably, the distributing manner of the vacuum suspension smelting in the step (1) is as follows: uniformly covering the nickel material on the upper part of the titanium material at the bottom of the crucible, and uniformly mixing the nickel material and the titanium material on the upper part of the crucible;
the melting point of nickel is lower than that of titanium, the specific gravity of nickel is one time of that of titanium (Ni 8.9, ti 4.5), segregation is easy to generate, and the method for distributing materials in a crucible in sense induction smelting is very important.
Preferably, the conditions of the vacuum suspension smelting are: vacuum degree is less than 1Pa; the smelting current changes to: refining the rated current I1/3-1/2-3-1/4 for 30min; the casting temperature is the melting point +80-150 ℃.
The vacuum suspension smelting comprises the following specific steps: weighing nickel-titanium materials by a balance, distributing a crucible, closing a furnace door for vacuumizing, transmitting power for smelting, completely smelting, refining, reducing power and adjusting the temperature of molten metal, casting ingots, cooling by a vacuum furnace, breaking the ingots at normal temperature for discharging, pulling out the ingots, and analyzing components for later use.
Preferably, the smelting conditions of the vacuum consumable arc smelting are as follows: the vacuum degree is less than 1Pa, the smelting voltage is 20-40V, and the smelting current is 10000-18000A.
Preferably, the specific steps of vacuum consumable arc melting in the step (1) are as follows: preparing consumable electrode block by vacuum induction furnace ingot casting, assembling and welding vacuum consumable electrode, clamping the vacuum consumable electrode into consumable furnace electrode rod, guan Lumen, and vacuumizing (vacuum)The air degree is more than 3 multiplied by 10 -3 Millimeter mercury column), power transmission melting, adjusting the temperature and pressure flow of a smelting current and a crucible cooling water, continuously smelting, controlling the cooling speed of the ingot by electromagnetic stirring, reducing the smelting current, adjusting the size of shrinkage cavities and impurity distribution of the ingot, compensating shrinkage cavities, finishing smelting, controlling the cooling water temperature of a water-cooled copper crucible, simultaneously filling argon into a furnace for rapidly cooling the ingot, cooling the ingot along with the furnace, breaking vacuum at room temperature, discharging the ingot, peeling the ingot, removing shrinkage cavities, and analyzing components for standby.
The nickel-titanium alloy is further purified by high vacuum smelting, and the components of the nickel-titanium alloy are completely homogenized; meanwhile, the size and distribution state of ingot casting tissues and a very small amount of nonmetallic impurities are controlled by controlling the cooling speed of the water-cooled copper crucible.
Preferably, the hot working process in the step (2) sequentially comprises ingot forging and billet opening, hot rolling and grain structure refinement control;
wherein, the parameters of the ingot casting forging blank opening are as follows: the cogging heating temperature is 950-1050 ℃, the forging temperature is 980-1020 ℃, the heat preservation time is 30-60min, and the dimension after forging is phi 120-130mm;
the parameters of the hot rolling are as follows: the rolling temperature is 950-1000 ℃, and the deformation size is phi 120-130 mm-phi 6.0mm; the hot rolling is one of the most important control links for ensuring the performance of the nickel-titanium alloy, and the refinement of grain structures can be ensured only by processing the ultrahigh deformation rate at a higher temperature;
grain structure refinement control includes: drawing with large deformation rate and rapidly cooling; the parameters of the large deformation ratio drawing are as follows: the processing temperature is 550-650 ℃, the drawing time is less than 1min, and the processing size is phi 6.0-phi 3.0mm; the intensity of the rapid cooling is more than 230 ℃/s and the time is less than 5s.
Preferably, the cold drawing deformation size of the wire drawing in the step (2) is phi 3.0-1.0-0.30 mm, the wire drawing linear speed is 1000-1500mm/min, the annealing temperature is 400-450 ℃, and the temperature is kept for 10-15min.
Preferably, the surface treatment in step (2) is ultrasonic cleaning with alcohols.
The production device of the production method of the medical nickel-titanium alloy wire comprises a vacuum electron beam melting furnace, a water-cooled copper crucible vacuum induction suspension melting furnace, a vacuum consumable arc furnace, first heating equipment, hot forging equipment, second heating equipment, a hot rolling mill, a first wire drawing machine, a second wire drawing machine and cleaning equipment which are connected in sequence.
Preferably, the first heating device and the second heating device use resistance furnaces.
Preferably, the second wire drawing machine.
Compared with the prior art, the invention has the following beneficial effects:
the invention starts from the basic process of nickel-titanium alloy wire production, comprehensively improves the existing process method in the aspects of component precise control technology, ingot smelting process method, hot working process, heat treatment process and tissue property adjustment control, improves the uniformity, stability and consistency of nickel-titanium alloy wire products, and lays a good foundation for the production of high-level medical devices.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described, and the drawings in the description are only embodiments of the present invention.
FIG. 1 is a schematic diagram of a distribution method of vacuum suspension smelting according to example 1 of the present invention, wherein 1 is purified titanium and 2 is purified nickel.
Detailed Description
The following describes embodiments of the invention, examples of which are illustrated in the accompanying drawings and described with reference to the drawings are intended to be illustrative of the invention and not to be construed as limiting the invention, as the invention employs equipment which is conventional in the art and which is available for direct purchase.
The production device of the medical nickel-titanium alloy wire comprises a vacuum electron beam melting furnace, a water-cooled copper crucible vacuum induction suspension melting furnace, a vacuum consumable arc furnace, first heating equipment, hot forging equipment, second heating equipment, a hot rolling mill, a first wire drawing machine, a second wire drawing machine and cleaning equipment which are connected in sequence;
the first heating device and the second heating device are resistance furnaces;
the second wire drawing machine is a box wire drawing machine, the number of the dies is 15-20, and the size diameter is 3.0-0.3mm;
example 1
The production method for producing the medical nickel-titanium alloy wire by adopting the production device specifically comprises the following steps:
(1) Purifying: the raw materials are electrolytic nickel (Ni > 99.3%) with grade more than 1 and sponge titanium (Ti > 99.5%) with grade more than 0, respectively placing nickel material and titanium material into vacuum electron beam furnace box, sealing furnace door, vacuumizing, vacuum degree is > 1×10 -3 Millimeter mercury column, and power transmission smelting;
nickel: the smelting process is repeated from heating to melting to cooling at about 1453 ℃ of nickel melting point between 1400-2450 ℃ for more than three times, so that gas and impurity elements are continuously evaporated and removed, the purity of nickel is purified from 2N5 to 4N5 (99.5% -99.995%), the nickel is discharged from a furnace, and an electrolytic nickel plate is sheared into blocks with the size of 20-30mm to be used as smelting raw materials for standby;
titanium: the melting point of titanium is about 1668 ℃, the smelting is repeatedly carried out between 1600-2800 ℃ and the process of heating, melting, cooling and refining is carried out for more than three times, so that gas and impurity elements are continuously evaporated and removed, the purity of titanium is purified from 2N5 to 4N5 (99.5% -99.995%), and the titanium is discharged from a furnace, is titanium sponge, and has the granularity of 0.8-3.0mm for standby;
after electron beam melting, nickel titanium cast ingots are rolled to be used as raw materials for induction furnaces.
(2) Carrying out vacuum suspension smelting and vacuum consumable arc smelting on the purified nickel material and titanium material to obtain an ingot;
wherein, the distribution mode of the vacuum suspension smelting is as shown in figure 1: because the specific gravity of titanium is 4.5, the specific gravity of nickel is 8.9, the specific gravity of nickel is great, the specific gravity of titanium is small, the segregation of specific gravity is prevented, the bottom of the crucible is horizontally layered, the purified nickel material 2 is uniformly covered on the upper part of the purified titanium material 2, the purified nickel material 2 and the purified titanium material 1 are mixed on the upper part of the crucible by adopting a vertical nickel-titanium mixed distribution method, the nickel-titanium interval distribution on the upper part of the crucible can be melted firstly after the bottom material is melted, and the titanium-nickel material on the upper part of the crucible is slowly lowered into a molten pool to be melted simultaneously, so that the basic alloying consistency is ensured, and the melting process of the vacuum induction suspension smelting furnace of the water-cooled copper crucible is specifically as follows:
weighing nickel-titanium material by a balance (weighing error is less than 0.01 g), distributing a crucible, vacuumizing a furnace door (vacuum degree is less than 1 Pa), transmitting power for smelting (smelting current change: rated current is 1/3 < -1/2 > -1 < -2 > -3 < -1/4 >), completely smelting, refining (30 min), reducing power, regulating metal liquid temperature, casting an ingot (the temperature is the melting point of +80-150 ℃), cooling a vacuum furnace, breaking the ingot at normal temperature, discharging the ingot from the furnace, pulling a cast ingot skin (phi 10-25mm bar), analyzing components and reserving;
the vacuum consumable arc furnace smelting process specifically comprises the following steps:
the consumable electrode block (argon shielded welding consumable electrode, smelting current 8000-19000A, voltage 20-40V), assembly welding vacuum consumable electrode, clamping vacuum consumable electrode into consumable furnace electrode rod Guan Lumen, vacuumizing (vacuum degree > 3×10) -3 Millimeter mercury) to power on and melting, adjusting smelting current (the smelting process is to firstly perform one third of rated current in 5min, then continuously adding current to about 80% of rated current, keeping unchanged, reducing current to 50% -40% -30% -10% in 10min after smelting is finished), controlling cooling speed of the ingot by continuously smelting electromagnetic stirring, reducing smelting current to adjust size of shrinkage cavity and impurity distribution of the ingot, compensating shrinkage cavity, finishing smelting, controlling cooling water temperature of a water-cooled copper crucible, simultaneously filling argon gas into the furnace for rapid cooling of the ingot, cooling the ingot along with the furnace, breaking vacuum at room temperature, discharging the ingot, skinning the ingot, removing shrinkage cavity, analyzing components and reserving;
(3) Sequentially carrying out hot processing, wire drawing and surface treatment on the cast ingot to obtain a medical nickel-titanium alloy wire;
the hot working process comprises the following specific steps:
1) Ingot forging cogging
Heating the cast ingot by a resistance furnace, free forging, cogging, crushing the cast ingot casting structure, sawing and blanking according to technical requirements after primary forging, secondarily heating, upsetting and forging for more than 3 times in each direction to obtain hot-rolled blanks with phi of 120-130mm, and removing surface oxide skin through cold working;
cogging heating temperature: 950-1050 ℃;
forging temperature: 980-1020 ℃;
the heat preservation time is 30-60min;
2) Hot rolling
Heating is carried out by a resistance furnace, and hot rolling is carried out by a high-linear-speed high-precision hot rolling mill;
rolling temperature: 950-1000 DEG C
Deformation dimensions: phi 120-phi 6.0mm (primary heating, multi-pass rolling forming and air cooling);
3) Grain structure refinement drawing
Processing is carried out on an argon-blowing quick-cooling continuous first wire drawing machine;
the processing size range is as follows: phi 6.0-phi 3.0mm
Drawing time is less than 1min
Processing temperature: 550-650 DEG C
Cooling strength: 230 ℃/S for less than 5S;
4) Wire drawing
A plurality of wire drawing dies are arranged in the box body, the wire drawing dies are made of tungsten nickel hard alloy, the wire drawing linear speed is controlled by a computer and can be controlled by the speed, the lubricant is phosphate emulsifier (40 percent of phosphate, 2-3 percent of sodium stearate and the balance of water), the machining principle is that the diameter phi is about 3.0mm, the wire drawing dies are continuously deformed and machined through a plurality of dies arranged in the box body, the nickel titanium alloy wire with the required size specification is sent out from a wire outlet,
cold drawing deformation size range:
phi 3.0-1.0 mm (Nickel-titanium alloy wire)
Phi 1.0-0.30 mm (Nickel-titanium alloy wire)
Linear velocity: 1000-1500mm/min
Annealing temperature: 400-450 ℃;
5) Surface treatment: ultrasonically cleaning the surface of the nickel-titanium alloy wire by adopting alcohols (50% of methanol, 20% of ethanol and the balance of water), wherein the power is 10-30KW, and the ultrasonic time is 10-20min;
the performance data of products with different specifications and sizes prepared by adopting the preparation method provided by the invention are as follows:
(1) nickel-titanium alloy wire
The components are as follows: ni 50% (atomic percent)
The main production process parameters are as follows:
cogging heating temperature: 950 ℃;
forging temperature: 980 ℃.
The heat preservation time is as follows: 30min;
pier drawing forging temperature: 980 ℃.
Hot rolling heating temperature: 1020 ℃;
rolling temperature: 980 ℃.
Deformation dimensions: phi 120-phi 6.0mm;
heat treatment temperature: 580 deg.C;
the heat preservation time is as follows: 30min.
The processing size range is as follows: phi 6.0-phi 3.0mm;
processing temperature: 550 ℃;
cooling strength: 230 ℃ C./S, time is 4S.
Linear velocity: linear velocity: 1000 mm/min
Annealing temperature: 400 ℃;
the ultrasonic cleaning power is 10KW, and the ultrasonic time is 10min;
phase transition point: ms 61 ℃ As 79 ℃ (electronic differential instrument, national institute of sciences metal standard detection) specification phi 2.0mm
Mechanical properties (annealed state):
σb 910MPa
δ55％；
(2) nickel-titanium alloy wire
The main production process parameters are as follows:
cogging heating temperature: 1020 ℃;
forging temperature: 1000 ℃;
pier drawing forging temperature: 990 ℃.
Hot rolling heating temperature: 1010 ℃;
rolling temperature: 980 ℃.
Deformation dimensions: phi 120-phi 6.0mm;
heat treatment temperature: 590 ℃;
the heat preservation time is as follows: 30min.
The processing size range is as follows: phi 6.0-phi 3.0mm;
processing temperature: 600 ℃;
cooling strength: 230 ℃ C./S, time is 4S.
Linear velocity: 1500 mm/min;
annealing temperature: 400 ℃;
the ultrasonic cleaning power is 10KW, and the ultrasonic time is 10min;
the components are as follows: ni 51% (atomic percent)
Phase transition point: ms-31deg.C As-13deg.C
Specification phi 0.5mm
Mechanical properties (annealed state):
σb 890MPa
δ62％；
from the above, the prepared product has excellent mechanical properties and high plasticity in a state of higher strength.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The production method of the medical nickel-titanium alloy wire is characterized by comprising the following steps of;
(1) Carrying out vacuum suspension smelting and vacuum consumable arc smelting on the purified nickel material and titanium material to obtain an ingot;
(2) And (3) sequentially carrying out a thermal processing technology, wire drawing and surface treatment on the cast ingot to obtain the medical nickel-titanium alloy wire.
2. The method of producing a medical nickel-titanium alloy wire according to claim 1, wherein the purity of the nickel and titanium materials in step (1) is 4N5;
the purification method is characterized in that the nickel material and the titanium material are respectively smelted and purified by adopting vacuum electron beams, and the specific steps are as follows:
nickel material: repeatedly melting, cooling and refining the nickel material for at least three times at 1400-2450 ℃;
titanium material: and (3) repeatedly melting, cooling and refining the titanium material for at least three times at 1600-2800 ℃.
3. The method for producing a medical nickel-titanium alloy wire according to claim 1, wherein the vacuum suspension smelting in the step (1) is performed in a material distribution manner of: uniformly covering the nickel material on the upper part of the titanium material at the bottom of the crucible, and uniformly mixing the nickel material and the titanium material on the upper part of the crucible;
the conditions of the vacuum suspension smelting are as follows: vacuum degree is less than 1Pa; the smelting current changes to: refining the rated current I1/3-1/2-3-1/4 for 30min; the casting temperature is the melting point +80-150 ℃.
4. The method for producing a medical nickel-titanium alloy wire according to claim 1, wherein the conditions for melting the vacuum consumable arc melting in step (1) are: the vacuum degree is less than 1Pa, the smelting voltage is 20-40V, and the smelting current is 10000-18000A.
5. The method for producing a medical nickel-titanium alloy wire according to claim 1, wherein the hot working process in the step (2) comprises ingot forging and billet opening, hot rolling and grain structure refinement control in sequence;
wherein, the parameters of the ingot casting forging blank opening are as follows: the cogging heating temperature is 950-1050 ℃, the forging temperature is 980-1020 ℃, the heat preservation time is 30-60min, and the dimension after forging is phi 120-130mm;
the parameters of the hot rolling are as follows: the rolling temperature is 950-1000 ℃, and the deformation size is phi 120-130 mm-phi 6.0mm;
grain structure refinement control includes: drawing with large deformation rate and rapidly cooling; the parameters of the large deformation ratio drawing are as follows: the processing temperature is 550-650 ℃, the drawing time is less than 1min, and the processing size is phi 6.0-phi 3.0mm; the intensity of the rapid cooling is more than 230 ℃/s and the time is less than 5s.
6. The method for producing the medical nickel-titanium alloy wire according to claim 1, wherein the cold drawing deformation size of the drawing wire in the step (2) is phi 3.0-1.0-0.30 mm, the linear speed of the drawing wire is 1000-1500mm/min, the annealing temperature is 400-450 ℃, and the temperature is kept for 10-15min.
7. The method of producing a medical nitinol wire according to claim 1, wherein the surface treatment in step (2) is ultrasonic cleaning with alcohols.
8. The apparatus for producing a medical nickel-titanium alloy wire according to any one of claims 1 to 7, comprising a vacuum electron beam melting furnace, a water-cooled copper crucible vacuum induction suspension melting furnace, a vacuum consumable arc furnace, a first heating device, a hot forging device, a second heating device, a hot rolling mill, a first wire drawing machine, a second wire drawing machine and a cleaning device which are connected in this order.
9. The production apparatus according to claim 8, wherein the first heating device and the second heating device employ resistance furnaces.
10. The production device according to claim 8, wherein the second wire drawing machine is a box wire drawing machine, the number of the dies is 15-20, and the dimension diameter is 3.0-0.3mm.
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| CN202311096003.5A CN117144166A (en) | 2023-08-29 | 2023-08-29 | Production method and production device of medical nickel-titanium alloy wire |
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