CN117753810A - Preparation method of high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube - Google Patents
Preparation method of high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube Download PDFInfo
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- CN117753810A CN117753810A CN202311845168.8A CN202311845168A CN117753810A CN 117753810 A CN117753810 A CN 117753810A CN 202311845168 A CN202311845168 A CN 202311845168A CN 117753810 A CN117753810 A CN 117753810A
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- memory alloy
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- 229910001000 nickel titanium Inorganic materials 0.000 title claims abstract description 26
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910001285 shape-memory alloy Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000010622 cold drawing Methods 0.000 claims abstract description 33
- 238000005554 pickling Methods 0.000 claims abstract description 17
- 238000003754 machining Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 32
- 230000009467 reduction Effects 0.000 claims description 24
- 230000008569 process Effects 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 238000000137 annealing Methods 0.000 description 11
- 229910001369 Brass Inorganic materials 0.000 description 9
- 239000010951 brass Substances 0.000 description 9
- 238000000227 grinding Methods 0.000 description 9
- 238000005520 cutting process Methods 0.000 description 8
- 238000005242 forging Methods 0.000 description 7
- 238000003723 Smelting Methods 0.000 description 6
- 230000003746 surface roughness Effects 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000005476 size effect Effects 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 229910004337 Ti-Ni Inorganic materials 0.000 description 1
- 229910011209 Ti—Ni Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- KHYBPSFKEHXSLX-UHFFFAOYSA-N iminotitanium Chemical compound [Ti]=N KHYBPSFKEHXSLX-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000006386 memory function Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Metal Extraction Processes (AREA)
Abstract
The invention discloses a preparation method of a high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube, which comprises the following steps: step 1: the bar is made into a tube blank through pulse perforation and wire-cut electric discharge machining, and the tube blank is pickled in pickling solution; step 2: drawing the tube blank for 2-10 times by adopting die-free drawing; step 3: drawing the tube blank for 1 time by adopting cold drawing; step 4: drawing the tube blank for 1-2 times by adopting die-free drawing; step 5: drawing the tube blank for 1 time by adopting cold drawing to obtain a finished capillary; the invention adopts the combination of the dieless drawing and the cold drawing, can greatly improve the traditional drawing efficiency and obtain the nickel-titanium capillary with high dimensional accuracy.
Description
Technical Field
The invention belongs to the field of material processing, and particularly relates to a preparation method of a high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube.
Background
The Ti-Ni shape memory alloy is an important functional material with excellent shape memory function, superelasticity, good corrosion resistance and biocompatibility. Since the early discovery of the 60 s of the 20 th century, the polymer has been widely used in various fields such as aerospace, electronics and medical treatment. At present, only a few countries or companies in the world have the production capacity of nickel-titanium shape memory alloy capillaries and realize industrialization. The domestic Beijing nonferrous metal institute, shenyang metal institute, well-known universities and certain civil enterprises are also actively developing.
Extrusion and drawing are the main methods of preparing nickel-titanium shape memory alloy capillaries. The extrusion process is mainly divided into three types: the extrusion process is suitable for producing nickel-titanium alloy pipes with larger specifications, the reverse drawing process is suitable for producing nickel-titanium capillaries with small specifications, the traditional pipe die drawing can be divided into fixed core head drawing, floating core head drawing, core die drawing and coreless die drawing, but the traditional pipe die drawing is not suitable for preparing capillaries with high precision, on one hand, the core rod is difficult to insert in the pipe by the core drawing, on the other hand, due to the miniaturized size effect, the friction resistance between the die and the pipe is increased, and the forming limit is reduced.
The problems of multiple drawing passes and low efficiency in the prior art are that the deformation of the pipe in each pass is about 10% in the prior art, and the whole drawing number is more than 30 times, so that at least 15 times of intermediate annealing are needed for preparing the capillary, and the drawing efficiency is low.
Disclosure of Invention
The invention aims to provide a preparation method of a nickel-titanium shape memory alloy capillary tube with high precision and high efficiency, which aims to solve the problems of multiple drawing times, low forming limit and low efficiency required by pipe drawing in the prior art.
The invention adopts the following technical scheme: a preparation method of a high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube comprises the following steps:
step 1: the bar is made into a tube blank through pulse perforation and wire-cut electric discharge machining, and the tube blank is pickled in pickling solution;
step 2: drawing the tube blank for 2-10 times by adopting die-free drawing;
step 3: drawing the tube blank for 1 time by adopting cold drawing;
step 4: drawing the tube blank for 1-2 times by adopting die-free drawing;
step 5: drawing the tube blank for 1 time by adopting cold drawing to obtain a finished capillary;
wherein the outer diameter of the finished capillary tube is smaller than 1mm, the wall thickness is 0.02-1 mm, and the length is 1-2 m.
Further, the tube blank raw materials in the step 1 comprise the following components in percentage by weight: ni:54 to 57wt% and the balance Ti.
Further, the pickling temperature in the step 1 is 50-80 ℃, and the pickling time is 30-60 min.
Further, the heating temperature in the drawing process in the step 2 and the step 4 is 700-950 ℃, the drawing speed is 5-15 mm/min, and the single-pass surface reduction rate is 30-50%.
Further, the single-pass reduction ratio in the drawing process in the step 3 and the step 5 is less than 5%, and the cold drawn pipe is annealed and straightened at the speed of 2m/min at the temperature of 400-600 ℃.
Further, the dieless drawing in steps 2 and 4 uses a rod-shaped tungsten steel as the non-deformable core.
Further, cold drawing in steps 3 and 5 employs a deformable Huang Tongxin.
The beneficial effects of the invention are as follows:
the invention adopts the combination of the dieless drawing and the cold drawing, can greatly improve the traditional drawing efficiency and obtain the nickel-titanium capillary with high dimensional accuracy;
the invention adopts the non-deformable core to draw the tube blank for 2-10 times without die drawing, the reduction ratio of each pass is 30-50%, the tube can be rapidly drawn to smaller size and wall thickness, but because the outer surface of the tube is rough after the non-deformable core is drawn without die drawing, the dimensional accuracy is low, the tube blank is drawn for 1 time after the non-die drawing, at this time, the outer wall of the tube is greatly improved due to the constraint surface roughness and dimensional accuracy of the die, and the dimension and the surface of the tube can be prevented from being directly realized through final cold drawing when the tube is finished by introducing cold drawing in the middle;
the tube blank is drawn for 1-2 times by adopting the die-free drawing after the intermediate cold drawing, the tube blank can be drawn to be close to the size of a finished product again and rapidly, but the roughness and the dimensional precision of the outer surface of the tube blank are slightly reduced after the die-free drawing for 1-2 times, and finally the tube blank is drawn for 1 time by adopting the cold drawing to obtain the finished capillary tube, so that the dimensional precision and the surface roughness of the outer wall of the tube are improved, and the quality and the dimensional precision of the inner surface and the outer surface of the whole capillary tube finished product are well ensured due to the introduction of the intermediate cold drawing. Therefore, the invention improves the dimensional accuracy and the surface roughness of the pipe by introducing the die drawing in the middle and the final stage of the multipass die-free belt core drawing;
according to the invention, the core rod is hard alloy in the non-deformable core die-free drawing process, the inner diameter size of the pipe is basically unchanged, and the deformable brass core die is selected in the die drawing process, so that the inner diameter and the outer diameter of the pipe brass core rod and the nickel-titanium shape memory alloy pipe cooperatively deform in the drawing process, and the reduction of the overall size of the pipe is realized.
Drawings
FIG. 1 is a transverse low magnification photograph of a capillary tube prepared as described in example 1 of the present invention;
FIG. 2 is a longitudinal low magnification photograph of a capillary tube prepared as described in example 1 of the present invention.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention discloses a preparation method of a high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube, which comprises the following steps:
step 1: pressing raw materials into electrode blocks, welding, and smelting into cast ingots by a vacuum consumable smelting furnace; homogenizing, heating, forging and grinding to obtain forging stock; heating, rolling, cutting off, grinding and sizing to obtain a rolled rod; the bar is manufactured after the roller type rough straightening, peeling, annealing, roller type fine straightening, grinding, polishing and flat head; the bar is made into a tube blank through pulse perforation and wire-cut electric discharge machining, and the tube blank is pickled in pickling solution. After electric spark cutting, the inner wall surface of the pipe always generates some residues and cutting marks, and the residues and the cutting marks can be removed by acid washing, so that the inner wall of the pipe is bright, and the subsequent processing is facilitated.
Step 2: drawing the tube blank for 2-10 times by adopting die-free drawing;
step 3: drawing the tube blank for 1 time by adopting cold drawing;
step 4: drawing the tube blank for 1-2 times by adopting die-free drawing;
step 5: drawing the tube blank for 1 time by adopting cold drawing to obtain a finished capillary;
wherein the outer diameter of the finished capillary tube is smaller than 1mm, the wall thickness is 0.02-1 mm, and the length is 1-2 m.
Wherein, the raw materials of the tube blank in the step 1 comprise the following components in percentage by weight: ni:54 to 57wt% and the balance Ti. The pickling temperature in the step 1 is 50-80 ℃ and the pickling time is 30-60 min.
Wherein, the heating temperature in the drawing process in the step 2 and the step 4 is 700-950 ℃, the drawing speed is 5-15 mm/min, and the single-pass surface reduction rate is 30-50%.
Wherein, the single-pass reduction ratio in the drawing process in the step 3 and the step 5 is less than 5 percent, and the cold drawn pipe is annealed and straightened at the speed of 2m/min at the temperature of 400-600 ℃.
Wherein, the dieless drawing in steps 2 and 4 uses rod-shaped tungsten steel as the non-deformable core.
Wherein, the cold drawing in steps 3 and 5 adopts a deformable Huang Tongxin.
Compared with the cold drawing with a die, namely the cold drawing with a die, the cold drawing with a die has the advantages of large area reduction, no die, no friction, flexible process, high efficiency and the like, however, in the process of processing the micro-fine pipe, the cold drawing with a die has considerable problems, namely the dimensional accuracy of the pipe in the process of drawing the product with a die is low, and the surface roughness is large.
The traditional deformable brass core mold has small reduction ratio when cold drawing the pipe, usually about 10% of deformation amount of each pass, so that a plurality of passes and intermediate annealing are needed for preparing the capillary, drawing efficiency is lower, friction resistance between a cutter and the capillary is increased due to the microminiaturization size effect, forming limit is reduced, but compared with the cold drawing of the deformable brass core mold, the cold drawing of the deformable brass core mold has high surface quality and dimensional accuracy of a finished pipe due to the restraint of a mold.
The non-deformable core die-free drawing has the advantages that the reduction ratio of more than 30% can be obtained only through a plurality of passes, and the drawing efficiency can be improved by at least 50%; and because of the existence of the non-deformable core, the dimensional accuracy of the inner surface of the pipe is high and the roughness is low, however, the non-deformable core is pulled out without a mould, and the dimensional accuracy of the outer surface of the pipe is low and the surface roughness is large.
Therefore, in order to obtain the high-precision nickel-titanium shape memory alloy capillary tube with high efficiency, the invention proposes that firstly, the non-deformable core is adopted to draw the tube blank for 2-10 times without a die, the reduction rate of each pass is 30-50%, the tube can be rapidly drawn to smaller size and wall thickness, but because the outer surface of the tube is rough after the non-deformable core is adopted to draw the tube blank without the die, the dimensional precision is low, the cold drawing is adopted to draw the tube blank for 1 time after the non-die drawing, at the moment, the roughness and the dimensional precision of the outer wall of the tube can be greatly improved due to the constraint surface of a die, and the dimension and the surface of the tube can be avoided from being directly realized through the final cold drawing when the tube is finished by introducing cold drawing in the middle. The tube blank is drawn for 1-2 times by adopting the dieless drawing after the intermediate cold drawing, the tube blank can be drawn to be close to the size of a finished product again and rapidly, but the roughness and the dimensional precision of the outer surface of the tube blank are slightly reduced after the dieless drawing for 1-2 times. Therefore, the invention improves the dimensional accuracy and the surface roughness of the pipe by introducing the die drawing in the middle and the final stage of the multipass die-free belt core drawing.
The preparation method of the alloy capillary tube comprises the following steps:
step 1: pressing raw materials into electrode blocks, welding, and smelting into cast ingots with phi 400-420 mm by a vacuum consumable smelting furnace; homogenizing cast ingots with phi of 400-420 mm, heating, forging and grinding to prepare forging billets with phi of 100-150 mm; heating, rolling, cutting, grinding and sizing the forging stock with the diameter of 100-150 mm to obtain a rolled rod with the diameter of 10-20 mm; rolling bars with the diameter of phi 10-20 mm, carrying out roller rough straightening, peeling, annealing, roller fine straightening, grinding, polishing and flat head to prepare bars with the diameter of phi 9-18 mm; and (3) carrying out spark-perforating and linear cutting on the bar with the diameter phi of 9-18 mm to prepare a tube blank with the inner diameter phi of 5-14 mm.
Step 2: the tube blank with the inner diameter phi of 5-14 mm is drawn for 2-10 times in a non-mould way, so as to ensure the drawing efficiency, the heating temperature in the drawing process is 700-950 ℃, the drawing speed is 5-15 mm/min, and the single-pass reduction rate is 30-50%.
Step 3: cold drawing for 1 time by adopting a deformable brass mandrel, wherein the single-pass reduction rate in the drawing process is less than 5%, and the temperature of the cold drawn pipe is as follows: annealing and straightening at 400-600 deg.c and 2 m/min.
Step 4: drawing the tube blank with the diameter of 5-10 mm for 1-2 times by adopting the die-free drawing of the non-deformable core, wherein the heating temperature in the drawing process is 700-950 ℃, the drawing speed is 5-15 mm/min, and the single-pass reduction rate is 30-50%.
Step 5: cold drawing for 1 time by adopting a deformable brass mandrel, wherein the single-pass reduction rate in the drawing process is less than 5%, and the temperature of the cold drawn pipe is as follows: annealing at 400-600 deg.c and 2m/min and straightening to obtain capillary with outer diameter smaller than 1mm and wall thickness 0.02-1 mm and length 1-2 m.
Example 1
The preparation method of the finished nickel-titanium capillary tube with the outer diameter of 0.33mm and the inner diameter of 0.24mm comprises the following steps:
step 1: pressing the raw materials into electrode blocks, welding, and smelting into cast ingots with phi 420mm by a vacuum consumable smelting furnace; homogenizing, heating, forging and grinding the cast ingot to prepare forging stock with the diameter of 100 mm; heating, rolling, cutting off, grinding and cutting to a fixed size to obtain a rolled rod with the diameter of 14 mm; the rolled bar is subjected to roller type rough straightening, peeling, annealing, roller type fine straightening, grinding, polishing and flat head to prepare a bar with phi 12 mm; the bar is subjected to pulse perforation and wire-cut electric discharge machining to prepare a tube blank with the outer diameter phi of 12mm and the inner diameter phi of 8mm, and the tube blank is pickled in pickling solution for 30min.
Step 2: the tube blank is drawn for 7 times without mould, the heating temperature in the drawing process is 800 ℃, the drawing speed is 8mm/min, and the single-pass face reduction rate is 45%.
Step 3: and cold drawing is carried out for 1 time by adopting a deformable brass mandrel, and the single-pass reduction rate in the drawing process is 3%. The cold drawn pipe is at the temperature: annealing and straightening at 500 ℃ and the speed of 2 m/min.
Step 4: and carrying out die-free drawing on the tube blank for 2 times, wherein the heating temperature in the drawing process is 800 ℃, the drawing speed is 8mm/min, and the single-pass reduction rate is 45%.
Step 5: and cold drawing is carried out for 1 time by adopting a deformable brass mandrel, and the single-pass reduction rate in the drawing process is 3%. The cold drawn pipe is at the temperature: annealing and straightening at 500 ℃ and 2m/min, and pickling in pickling solution for 60min to obtain a finished capillary tube with the outer diameter of 0.33mm, the inner diameter of 0.24mm and the length of 1 m.
As shown in fig. 1 and 2, fig. 1 is a transverse low-power photograph of a capillary tube prepared in the embodiment, and it can be seen that the prepared capillary tube has small wall thickness deviation and good concentricity; fig. 2 is a longitudinal low-magnification photograph of the capillary tube prepared in this example, and it can be seen that the nickel-titanium capillary tube with high quality inner surface is prepared and the longitudinal wall thickness is uniformly distributed.
Example 2
Preparation of a NiTi capillary having an outer diameter of 0.98mm and an inner diameter of 0.58mm the procedure was otherwise identical to that of example 1 except that:
step 1, preparing a bar with the diameter of 18 mm; and the bar is subjected to pulse perforation and wire-cut electric discharge machining to prepare a tube blank with the outer diameter phi 18mm and the inner diameter phi 14 mm.
The heating temperature in steps 2 and 4 was 950 ℃ and step 2 was drawn 7 times, step 4 was drawn 1 time, the drawing speed was 6mm/min, and the single pass reduction was 40%.
The single-pass face reduction rate in the steps 3 and 5 is 4%, and the temperature of the cold drawn pipe is 600 ℃; annealing and straightening at a speed of 2m/min, pickling in pickling solution for 60min to obtain the finished capillary tube with the outer diameter of 0.98mm, the inner diameter of 0.58mm and the length of 1.5 m.
Example 3
Preparation of a NiTi capillary having an outer diameter of 0.24mm and an inner diameter of 0.14mm the procedure of example 1 was otherwise followed except that:
step 1, preparing a bar with the diameter of 9 mm; and the bar is subjected to pulse perforation and wire-cut electric discharge machining to prepare a tube blank with the outer diameter phi 9mm and the inner diameter phi 5 mm.
The heating temperature in the steps 2 and 4 is 800 ℃, the step 2 is drawn for 6 times, the step 4 is drawn for 1 time, the drawing speed is 6mm/min, and the single-pass reduction ratio is 30%.
The single pass reduction in steps 3 and 5 is 4%, and the temperature of the cold drawn pipe is: annealing and straightening at 500 ℃ and the speed of 2m/min, pickling for 60min in pickling solution, and finally obtaining the finished capillary tube with the outer diameter of 0.24mm, the inner diameter of 0.14mm and the length of 2m.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (7)
1. The preparation method of the nickel-titanium shape memory alloy capillary tube with high precision and high efficiency is characterized by comprising the following steps:
step 1: the bar is made into a tube blank through pulse perforation and wire-cut electric discharge machining, and the tube blank is pickled in pickling solution;
step 2: drawing the tube blank for 2-10 times by adopting die-free drawing;
step 3: drawing the tube blank for 1 time by adopting cold drawing;
step 4: drawing the tube blank for 1-2 times by adopting die-free drawing;
step 5: drawing the tube blank for 1 time by adopting cold drawing to obtain a finished capillary;
wherein the outer diameter of the finished capillary tube is smaller than 1mm, the wall thickness is 0.02-1 mm, and the length is 1-2 m.
2. The method for preparing the high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube according to claim 1, wherein the tube blank raw material in the step 1 comprises the following components in percentage by weight: ni:54 to 57wt% and the balance Ti.
3. The method for preparing a high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube according to claim 1, wherein the pickling temperature in the step 1 is 50-80 ℃ and the pickling time is 30-60 min.
4. The method for preparing the high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube according to claim 1, wherein the heating temperature in the drawing process in the step 2 and the step 4 is 700-950 ℃, the drawing speed is 5-15 mm/min, and the single-pass surface reduction rate is 30-50%.
5. The method for preparing a high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube according to claim 1, wherein the single-pass reduction rate in the drawing process in the step 3 and the step 5 is less than 5%, and the cold drawn tube is annealed and straightened at a speed of 2m/min at a temperature of 400-600 ℃.
6. The method of preparing a high precision, high efficiency nickel titanium shape memory alloy capillary tube as defined in claim 1, wherein the die-free drawing in steps 2 and 4 uses a rod-shaped tungsten steel as the non-deformable core.
7. The method for preparing a high-precision and high-efficiency nickel-titanium shape memory alloy capillary tube according to claim 1, wherein cold drawing in steps 3 and 5 adopts deformable Huang Tongxin.
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