CN101722209B - Preparation method of large slenderness ratio and high-toughness magnesium alloy capillary - Google Patents
Preparation method of large slenderness ratio and high-toughness magnesium alloy capillary Download PDFInfo
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- CN101722209B CN101722209B CN2009100732691A CN200910073269A CN101722209B CN 101722209 B CN101722209 B CN 101722209B CN 2009100732691 A CN2009100732691 A CN 2009100732691A CN 200910073269 A CN200910073269 A CN 200910073269A CN 101722209 B CN101722209 B CN 101722209B
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 131
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 49
- 238000000137 annealing Methods 0.000 claims abstract description 20
- 238000001125 extrusion Methods 0.000 claims description 72
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 229910002804 graphite Inorganic materials 0.000 claims description 22
- 239000010439 graphite Substances 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- XTLNYNMNUCLWEZ-UHFFFAOYSA-N ethanol;propan-2-one Chemical compound CCO.CC(C)=O XTLNYNMNUCLWEZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000009413 insulation Methods 0.000 claims description 14
- 229960000583 acetic acid Drugs 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000012362 glacial acetic acid Substances 0.000 claims description 10
- 238000005554 pickling Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000001192 hot extrusion Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000010147 laser engraving Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- 210000005239 tubule Anatomy 0.000 description 1
- 238000000304 warm extrusion Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a large slenderness ratio and high-toughness magnesium alloy capillary, relating to a preparation method of a magnesium alloy capillary, and solving the problems of slower extruding speed, low production efficiency, poor performance, and grosser crystal grains of extruded bars and plates existing in a traditional method for preparing the magnesium alloy capillary. The method comprises the following steps of: firstly, manufacturing magnesium alloy extruded bars; secondly, manufacturing blanks for extruded capillaries; thirdly, manufacturing cylinders; fourthly, manufacturing extruded blanks; fifthly, manufacturing magnesium alloy extruded tubes; and seventhly, obtaining the large slenderness ratio and high-toughness magnesium alloy capillaries by carrying out annealing treatment and acidizing treatment on the magnesium alloy capillaries. The large slenderness ratio and high-toughness magnesium alloy capillaries obtained in the invention have uniform wall thickness, well-closed formation, high mechanical property, high elongation, tensile strength and yield strength which are measured under room temperature, fine crystal grains and large length. The invention has the advantages of high extruding speed, low cost, low consumed capacity, and greatly improved production efficiency.
Description
Technical field
The present invention relates to magnesium alloy preparation method capillaceous.
Background technology
In recent years, density is low, specific strength is big, rigidity is high because of magnesium alloy has, particularly have good biocompatibility, elastic modelling quantity characteristics low, that can progressively degrade and effectively be absorbed by human body in vivo, now increasing magnesium alloy materials is used to surgery implantation instrument such as hone lamella, nail, and after one's own heart Products Development and the clinical practice such as endovascular stent of internal medicine intervention apparatus.But the traditional diamond-making technique of magnesium alloy is hot machining, as hot-extrusion method, hot rolling system method and hot pull method, these methods all exist extrusion speed slower, production efficiency is low, poor performance (percentage elongation is lower than 10%), the problem of extrusion bar, sheet material crystal grain thicker (greater than 10 μ m), these defectives cause existing method preparation carefully to realize than big magnesium alloy tubule, capillary or silk material are extremely difficult.
Summary of the invention
The present invention exists extrusion speed slower in order to solve existing preparation magnesium alloy method capillaceous, and production efficiency is low, poor performance, extrusion bar, the thicker problem of sheet material crystal grain, and a kind of high-fineness ratio, the magnesium alloy with high strength and ductility preparation method capillaceous who provides.
Preparation high-fineness ratio, magnesium alloy with high strength and ductility method capillaceous realize according to the following steps: one, magnesium alloy ingot is heated to 200～450 ℃ and insulation processing 0.5～1h, push under the condition that be 2～64 in extrusion ratio then, extrusion die drift speed is 20～30mm/s, extruded bar from magnesium alloy; Two, be annealing in process 2～8h under 200～420 ℃ of conditions with extruded bar from magnesium alloy in temperature, intercepting length is the bar of 20～50mm then, must push the capillary blank; Three, will push capillary with blank one end be processed into a base thickness degree be 2～5mm, the tube dark 8～25mm, the tube internal diameter be the cylinder of Φ 13.6～Φ 13.9mm; Four, high-strength graphite is processed into cylinder, the diameter of cylinder is to carry out interference fit under the condition of 0.02～0.08mm at the magnitude of interference with the internal diameter of tube, carries out press fit arrangement then, extrusion blank; Five, earlier extrusion die is preheated to 450 ℃, then extrusion blank is heated to 100～350 ℃ and insulation processing 0.2～0.5h, push under the condition that then be 3～169, extrusion die drift speed is 20～30mm/s in extrusion ratio, magnesium alloy extruded tube material blank; Six, the magnesium alloy at intercepting magnesium alloy extruded tube material blank two ends exposes high-strength graphite, is that the lengthening drill bit of Φ 1.6～Φ 3.0mm is cleared up the high-strength graphite in the caliber with the aperture then, must magnesium alloy capillary tubing; Seven, be annealing in process 2～8h under 200～420 ℃ of conditions with magnesium alloy capillary tubing in temperature, put into acetone-ethanol solution then and carry out ultrasonic processing 0.2～1.5h, be that 10%～20% glacial acetic acid aqueous solution is carried out pickling 10～60s with mass concentration more then, promptly get high-fineness ratio, magnesium alloy with high strength and ductility capillary; The internal diameter unanimity of cylinder tube in the diameter of dark consistent, the cylinder of cylinder tube and the step 3 in cylinder and the step 3 in the step 4 wherein; In the step 7 in acetone-ethanol solution acetone mix by 1: 1 volume ratio with absolute ethyl alcohol.
The high-fineness ratio that the present invention obtains, magnesium alloy with high strength and ductility capillary wall thickness and even tissue and mechanical property height (percentage elongation is 12%～26%), at room temperature recording tensile strength is 190～290MPa, yield strength is 120～180MPa; Prepare high-fineness ratio in the present invention, in the magnesium alloy with high strength and ductility method capillaceous, magnesium alloy is in extrusion process under the three-dimensional compressive stress effect, tissue thinning effect is obvious, select and the control extrusion process parameters, and the size that changes graphite-filled thing, and good lubricating process in the extrusion process, make high-fineness ratio magnesium alloy warm extrusion compactibility capillaceous deformation technique be achieved, and then obtain especially plasticity index height of combination property, and be convenient to follow-up plastic working (drawing) or machining (as laser engraving) surface quality is good and dimensional accuracy is high high-fineness ratio magnesium alloy capillary.Adopt method of the present invention to obtain high-fineness ratio, magnesium alloy with high strength and ductility capillary crystal grain tiny (average grain size 2 μ m), outside dimension is that 0.1～0.5mm, length are greater than 300mm for Φ 1～Φ 4mm, wall thickness only.
The inventive method extrusion speed in whole extrusion process has all promoted 15%～30% than existing method; Employed equipment is simple among the present invention, cost is low; The raw material source is cheap, market can be buied, and greatly reduces production cost; Technical process is simple, processing ease, the ability that consumed are low, has improved the efficient of producing greatly.
Description of drawings
The magnesium alloy capillary tissue scanning electromicroscopic photograph that Fig. 1 obtains for existing hot-extrusion method, the high-fineness ratio that Fig. 2 obtains for the specific embodiment 29, magnesium alloy with high strength and ductility capillary tissue scanning electromicroscopic photograph.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: present embodiment prepares high-fineness ratio, magnesium alloy with high strength and ductility method capillaceous realizes according to the following steps: one, magnesium alloy ingot is heated to 200～450 ℃ and insulation processing 0.5～1h, push under the condition that be 2～64 in extrusion ratio then, extrusion die drift speed is 20～30mm/s, extruded bar from magnesium alloy; Two, be annealing in process 2～8h under 200～420 ℃ of conditions with extruded bar from magnesium alloy in temperature, intercepting length is the bar of 20～50mm then, must push the capillary blank; Three, will push capillary with blank one end be processed into a base thickness degree be 2～5mm, the tube dark 8～25mm, the tube internal diameter be the cylinder of Φ 13.6～Φ 13.9mm; Four, high-strength graphite is processed into cylinder, the diameter of cylinder is to carry out interference fit under the condition of 0.02～0.08mm at the magnitude of interference with the internal diameter of tube, carries out press fit arrangement then, extrusion blank; Five, earlier extrusion die is preheated to 450 ℃, then extrusion blank is heated to 100～350 ℃ and insulation processing 0.2～0.5h, push under the condition that then be 3～169, extrusion die drift speed is 20～30mm/s in extrusion ratio, magnesium alloy extruded tube material blank; Six, the magnesium alloy at intercepting magnesium alloy extruded tube material blank two ends exposes high-strength graphite, is that the lengthening drill bit of Φ 1.6～Φ 3.0mm is cleared up the high-strength graphite in the caliber with the aperture then, must magnesium alloy capillary tubing; Seven, be annealing in process 2～8h under 200～420 ℃ of conditions with magnesium alloy capillary tubing in temperature, put into acetone-ethanol solution then and carry out ultrasonic processing 0.2～1.5h, be that 10%～20% glacial acetic acid aqueous solution is carried out pickling 10～60s with mass concentration more then, promptly get high-fineness ratio, magnesium alloy with high strength and ductility capillary; The internal diameter unanimity of cylinder tube in the diameter of dark consistent, the cylinder of cylinder tube and the step 3 in cylinder and the step 3 in the step 4 wherein; In the step 7 in acetone-ethanol solution acetone mix by 1: 1 volume ratio with absolute ethyl alcohol.
The specific embodiment two: the difference of the present embodiment and the specific embodiment one is that magnesium alloy ingot is AZ31 magnesium alloy ingot or MB15 magnesium alloy ingot in the step 1.Other step is identical with the specific embodiment one with parameter.
The specific embodiment three: present embodiment and the specific embodiment one or twos' difference is to be 10～45 in extrusion ratio in the step 1, to push under the condition that extrusion die drift speed is 22～28mm/s.Other step is identical with the specific embodiment one or two with parameter.
The specific embodiment four: present embodiment and the specific embodiment one or twos' difference is to be 30 in extrusion ratio in the step 1, to push under the condition that extrusion die drift speed is 25mm/s.Other step is identical with the specific embodiment one or two with parameter.
The specific embodiment five: the difference of the present embodiment and the specific embodiment one to four is in the step 1 magnesium alloy ingot to be heated to 250～400 ℃ also to be incubated processing 0.6～0.8h.Other step is identical with the specific embodiment one to four with parameter.
The specific embodiment six: the difference of the present embodiment and the specific embodiment one to four is in the step 1 magnesium alloy ingot to be heated to 300 ℃ also to be incubated processing 0.7h.Other step is identical with the specific embodiment one to four with parameter.
The specific embodiment seven: the difference of the present embodiment and the specific embodiment one to six is to be annealing in process 3～7h under 240～360 ℃ of conditions in temperature in the step 2.Other step is identical with the specific embodiment one to six with parameter.
The specific embodiment eight: the difference of the present embodiment and the specific embodiment one to six is to be annealing in process 4h under 300 ℃ of conditions in temperature in the step 2.Other step is identical with the specific embodiment one to six with parameter.
The specific embodiment nine: the difference of the present embodiment and the specific embodiment one to eight is that the length of intercepting bar in the step 2 is 30～40mm.Other step is identical with the specific embodiment one to eight with parameter.
The specific embodiment ten: the difference of the present embodiment and the specific embodiment one to eight is that the length of intercepting bar in the step 2 is 35mm.Other step is identical with the specific embodiment one to eight with parameter.
The specific embodiment 11: the difference of the present embodiment and the specific embodiment one to ten is that the tube base thickness degree of cylinder in the step 3 is that the internal diameter of 2.5～4.5mm, the dark 12～20mm of being of tube, tube is Φ 13.7～Φ 13.8mm.Other step is identical with the specific embodiment one to ten with parameter.
The specific embodiment 12: the difference of the present embodiment and the specific embodiment one to ten is that the tube base thickness degree of cylinder in the step 3 is that the dark internal diameter for 18mm, tube of 3mm, tube is Φ 13.75mm.Other step is identical with the specific embodiment one to ten with parameter.
The specific embodiment 13: the difference of the present embodiment and the specific embodiment one to 12 is that the magnitude of interference is 0.03～0.07mm in the step 4.Other step is identical with the specific embodiment one to 12 with parameter.
The specific embodiment 14: the difference of the present embodiment and the specific embodiment one to 12 is that the magnitude of interference is 0.05mm in the step 4.Other step is identical with the specific embodiment one to 12 with parameter.
The specific embodiment 15: the difference of the present embodiment and the specific embodiment one to 14 is to be 28～146 in extrusion ratio in the step 5, to push under the condition that extrusion die drift speed is 22～28mm/s.Other step is identical with the specific embodiment one to 14 with parameter.
The specific embodiment 16: the difference of the present embodiment and the specific embodiment one to 14 is to be 86 in extrusion ratio in the step 5, to push under the condition that extrusion die drift speed is 24mm/s.Other step is identical with the specific embodiment one to 14 with parameter.
The specific embodiment 17: the difference of the present embodiment and the specific embodiment one to 16 is in the step 5 extrusion blank to be heated to 150～300 ℃ also to be incubated processing 0.3～0.4h.Other step is identical with the specific embodiment one to 16 with parameter.
The specific embodiment 18: the difference of the present embodiment and the specific embodiment one to 16 is in the step 5 extrusion blank to be heated to 200 ℃ also to be incubated processing 0.35h.Other step is identical with the specific embodiment one to 16 with parameter.
The specific embodiment 19: the difference of the present embodiment and the specific embodiment one to 18 is that the lengthening drill bit aperture is Φ 1.8～Φ 2.6mm in the step 6.Other step is identical with the specific embodiment one to 18 with parameter.
The specific embodiment 20: the difference of the present embodiment and the specific embodiment one to 18 is that the lengthening drill bit aperture is Φ 2.4mm in the step 6.Other step is identical with the specific embodiment one to 18 with parameter.
The specific embodiment 21: the difference of the present embodiment and the specific embodiment one to 20 is to be annealing in process 4～6h under 240～360 ℃ of conditions in temperature.Other step is identical with the specific embodiment one to 20 with parameter.
The specific embodiment 22: the difference of the present embodiment and the specific embodiment one to 20 is to be annealing in process 5h under 300 ℃ of conditions in temperature.Other step is identical with the specific embodiment one to 20 with parameter.
The specific embodiment 23: the difference of the present embodiment and the specific embodiment one to 22 is that the mass concentration of glacial acetic acid aqueous solution in the step 7 is 12%～18%.Other step is identical with the specific embodiment one to 22 with parameter.
The specific embodiment 24: the difference of the present embodiment and the specific embodiment one to 22 is that the mass concentration of glacial acetic acid aqueous solution in the step 7 is 15%.Other step is identical with the specific embodiment one to 22 with parameter.
The specific embodiment 25: the difference of the present embodiment and the specific embodiment one to 24 be in the step 7 pickling time be 20～50s.Other step is identical with the specific embodiment one to 24 with parameter.
The specific embodiment 26: the difference of the present embodiment and the specific embodiment one to 24 be in the step 7 pickling time be 30s.Other step is identical with the specific embodiment one to 24 with parameter.
The specific embodiment 27: the difference of the present embodiment and the specific embodiment one to 26 be in the step 7 the ultrasonic processing time be 0.5～1.0h.Other step is identical with the specific embodiment one to 26 with parameter.
The specific embodiment 28: the difference of the present embodiment and the specific embodiment one to 26 be in the step 7 the ultrasonic processing time be 0.8h.Other step is identical with the specific embodiment one to 26 with parameter.
The specific embodiment 29: present embodiment prepares high-fineness ratio, magnesium alloy with high strength and ductility method capillaceous realizes according to the following steps: one, the AZ31 magnesium alloy ingot is heated to 220 ℃ and insulation processing 0.5h, push under the condition that be 10.56 in extrusion ratio then, extrusion die drift speed is 22mm/s, extruded bar from magnesium alloy; Two, be annealing in process 2h under 280 ℃ of conditions with extruded bar from magnesium alloy in temperature, intercepting is long then is the bar of 30mm, must push the capillary blank; Three, will push capillary with blank one end be processed into a base thickness degree be 5mm, the tube dark for 25mm, the tube an internal diameter be the cylinder of Φ 13.6mm; Four, high-strength graphite is processed into cylinder, the diameter of cylinder is to carry out interference fit under the condition of 0.05mm at the magnitude of interference with the internal diameter of tube, carries out press fit arrangement then, extrusion blank; Five, earlier extrusion die is preheated to 450 ℃, then extrusion blank is heated to 220 ℃ and insulation and handles 0.25h, push under the condition that then be 16, extrusion die drift speed is 22mm/s in extrusion ratio, magnesium alloy extruded tube material blank; Six, the magnesium alloy at intercepting magnesium alloy extruded tube material blank two ends exposes high-strength graphite, is that the lengthening drill bit of Φ 3.0mm is cleared up the high-strength graphite in the caliber with the aperture then, must magnesium alloy capillary tubing; Seven, be annealing in process 2h under 320 ℃ of conditions with magnesium alloy capillary tubing in temperature, put into acetone-ethanol solution then and carry out ultrasonic processing 0.5h, be that 10% glacial acetic acid aqueous solution is carried out pickling 25s with mass concentration more then, promptly get high-fineness ratio, magnesium alloy with high strength and ductility capillary; The internal diameter unanimity of cylinder tube in the diameter of dark consistent, the cylinder of cylinder tube and the step 3 in cylinder and the step 3 in the step 4 wherein; In the step 7 in acetone-ethanol solution acetone mix by 1: 1 volume ratio with absolute ethyl alcohol.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary are Φ 4.0 * 0.3mm.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary are 23% through recording percentage elongation, and at room temperature recording tensile strength is 240MPa, and yield strength is 150MPa.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary tissue scanning electromicroscopic photograph as shown in Figure 2, as can be seen from Figure 2 high-fineness ratio, magnesium alloy with high strength and ductility capillary surface crystal grain are tiny, even; And the magnesium alloy capillary tissue scanning electromicroscopic photograph that existing hot-extrusion method prepares as shown in Figure 1, as can be seen from Figure 1 magnesium alloy capillary surface grain size inequality.Comparison diagram 1 finds out obviously that with Fig. 2 high-fineness ratio, the magnesium alloy with high strength and ductility tissue surface capillaceous that present embodiment obtains obviously is better than the magnesium alloy capillary tissue surface that existing hot-extrusion method prepares.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary crystal grain tiny (average grain size 2 μ m).
The specific embodiment 30: present embodiment prepares high-fineness ratio, magnesium alloy with high strength and ductility method capillaceous realizes according to the following steps: one, the AZ31 magnesium alloy ingot is heated to 300 ℃ and insulation processing 0.5h, push under the condition that be 10.56 in extrusion ratio then, extrusion die drift speed is 20mm/s, extruded bar from magnesium alloy; Two, be annealing in process 4h under 400 ℃ of conditions with extruded bar from magnesium alloy in temperature, intercepting is long then is the bar of 30mm, must push the capillary blank; Three, will push capillary with blank one end be processed into a base thickness degree be 3mm, the tube dark 20mm, the tube internal diameter be the cylinder of Φ 13.9mm; Four, high-strength graphite is processed into cylinder, the diameter of cylinder is to carry out interference fit under the condition of 0.04mm at the magnitude of interference with the internal diameter of tube, carries out press fit arrangement then, extrusion blank; Five, earlier extrusion die is preheated to 450 ℃, then extrusion blank is heated to 200 ℃ and insulation and handles 0.25h, push under the condition that then be 28.4, extrusion die drift speed is 20mm/s in extrusion ratio, magnesium alloy extruded tube material blank; Six, six, the magnesium alloy at intercepting magnesium alloy extruded tube material blank two ends exposes high-strength graphite, is that the lengthening drill bit of Φ 2.8mm is cleared up the high-strength graphite in the caliber with the aperture then, must magnesium alloy capillary tubing; Seven, be annealing in process 2h under 280 ℃ of conditions with magnesium alloy capillary tubing in temperature, put into acetone-ethanol solution then and carry out ultrasonic processing 0.25h, be that 15% glacial acetic acid aqueous solution is carried out pickling 20s with mass concentration more then, promptly get high-fineness ratio, magnesium alloy with high strength and ductility capillary; The internal diameter unanimity of cylinder tube in the diameter of dark consistent, the cylinder of cylinder tube and the step 3 in cylinder and the step 3 in the step 4 wherein; In the step 7 in acetone-ethanol solution acetone mix by 1: 1 volume ratio with absolute ethyl alcohol.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary are Φ 3.0 * 0.2mm.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary are 15% through recording percentage elongation, and at room temperature recording tensile strength is 230MPa, and yield strength is 145MPa.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary crystal grain tiny (average grain size 2 μ m).
The specific embodiment 31: present embodiment prepares high-fineness ratio, magnesium alloy with high strength and ductility method capillaceous realizes according to the following steps: one, the MB15 magnesium alloy ingot is heated to 260 ℃ and insulation processing 0.5h, push under the condition that be 10.56 in extrusion ratio then, extrusion die drift speed is 22mm/s, extruded bar from magnesium alloy; Two, be annealing in process 3h under 220 ℃ of conditions with extruded bar from magnesium alloy in temperature, intercepting is long then is the bar of 30mm, must push the capillary blank; Three, will push capillary with blank one end be processed into a base thickness degree be 5mm, the tube dark 25mm, the tube internal diameter be the cylinder of Φ 13.6mm; Four, high-strength graphite is processed into cylinder, the diameter of cylinder is to carry out interference fit under the condition of 0.05mm at the magnitude of interference with the internal diameter of tube, carries out press fit arrangement then, extrusion blank; Five, earlier extrusion die is preheated to 450 ℃, then extrusion blank is heated to 220 ℃ and insulation and handles 0.4h, push under the condition that then be 16, extrusion die drift speed is 22mm/s in extrusion ratio, magnesium alloy extruded tube material blank; Six, six, the magnesium alloy at intercepting magnesium alloy extruded tube material blank two ends exposes high-strength graphite, is that the lengthening drill bit of Φ 3.0mm is cleared up the high-strength graphite in the caliber with the aperture then, must magnesium alloy capillary tubing; Seven, be annealing in process 2h under 320 ℃ of conditions with magnesium alloy capillary tubing in temperature, put into acetone-ethanol solution then and carry out ultrasonic processing 0.5h, be that 10% glacial acetic acid aqueous solution is carried out pickling 25s with mass concentration more then, promptly get high-fineness ratio, magnesium alloy with high strength and ductility capillary; The internal diameter unanimity of cylinder tube in the diameter of dark consistent, the cylinder of cylinder tube and the step 3 in cylinder and the step 3 in the step 4 wherein; In the step 7 in acetone-ethanol solution acetone mix by 1: 1 volume ratio with absolute ethyl alcohol.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary are Φ 4.0 * 0.3mm.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary are 21% through recording percentage elongation, and at room temperature recording tensile strength is 278MPa, and yield strength is 175Mpa.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary crystal grain tiny (average grain size 2 μ m).
The specific embodiment 32: present embodiment prepares high-fineness ratio, magnesium alloy with high strength and ductility method capillaceous realizes according to the following steps: one, the MB15 magnesium alloy ingot is heated to 350 ℃ and insulation processing 1h, push under the condition that be 10.56 in extrusion ratio then, extrusion die drift speed is 22mm/s, extruded bar from magnesium alloy; Two, be annealing in process 3h under 350 ℃ of conditions with extruded bar from magnesium alloy in temperature, intercepting is long then is the bar of 23mm, must push the capillary blank; Three, will push capillary with blank one end be processed into a base thickness degree be 3mm, the tube dark 20mm, the tube internal diameter be the cylinder of Φ 13.9mm; Four, high-strength graphite is processed into cylinder, the diameter of cylinder is to carry out interference fit under the condition of 0.02mm at the magnitude of interference with the internal diameter of tube, carries out press fit arrangement then, extrusion blank; Five, earlier extrusion die is preheated to 450 ℃, then extrusion blank is heated to 350 ℃ and insulation and handles 0.3h, push under the condition that then be 28.4, extrusion die drift speed is 22mm/s in extrusion ratio, magnesium alloy extruded tube material blank; Six, six, the magnesium alloy at intercepting magnesium alloy extruded tube material blank two ends exposes high-strength graphite, is that the lengthening drill bit of Φ 2.8mm is cleared up the high-strength graphite in the caliber with the aperture then, must magnesium alloy capillary tubing; Seven, be annealing in process 2h under 260 ℃ of conditions with magnesium alloy capillary tubing in temperature, put into acetone-ethanol solution then and carry out ultrasonic processing 1h, be that 10% glacial acetic acid aqueous solution is carried out pickling 15s with mass concentration more then, promptly get high-fineness ratio, magnesium alloy with high strength and ductility capillary; The internal diameter unanimity of cylinder tube in the diameter of dark consistent, the cylinder of cylinder tube and the step 3 in cylinder and the step 3 in the step 4 wherein; In the step 7 in acetone-ethanol solution acetone mix by 1: 1 volume ratio with absolute ethyl alcohol.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary are Φ 3.0 * 0.2mm.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary are 26% through recording percentage elongation, and at room temperature recording tensile strength is 328MPa, and yield strength is 254MPa.
The high-fineness ratio that present embodiment obtains, magnesium alloy with high strength and ductility capillary crystal grain tiny (average grain size 2 μ m).
Claims (10)
1. high-fineness ratio, magnesium alloy with high strength and ductility preparation method capillaceous, it is characterized in that preparing high-fineness ratio, magnesium alloy with high strength and ductility method capillaceous realizes according to the following steps: one, magnesium alloy ingot is heated to 200～450 ℃ and insulation and handles 0.5～1h, push under the condition that be 2～64 in extrusion ratio then, extrusion die drift speed is 20～30mm/s, extruded bar from magnesium alloy; Two, be annealing in process 2～8h under 200～420 ℃ of conditions with extruded bar from magnesium alloy in temperature, intercepting length is the bar of 20～50mm then, must push the capillary blank; Three, will push capillary with blank one end be processed into a base thickness degree be 2～5mm, the tube dark 8～25mm, the tube internal diameter be the cylinder of Φ 13.6～Φ 13.9mm; Four, high-strength graphite is processed into cylinder, the diameter of cylinder is to carry out interference fit under the condition of 0.02～0.08mm at the magnitude of interference with the internal diameter of tube, carries out press fit arrangement then, extrusion blank; Five, earlier extrusion die is preheated to 450 ℃, then extrusion blank is heated to 100～350 ℃ and insulation processing 0.2～0.5h, push under the condition that then be 3～169, extrusion die drift speed is 20～30mm/s in extrusion ratio, magnesium alloy extruded tube material blank; Six, the magnesium alloy at intercepting magnesium alloy extruded tube material blank two ends exposes high-strength graphite, is that the lengthening drill bit of Φ 1.6～Φ 3.0mm is cleared up the high-strength graphite in the caliber with the aperture then, must magnesium alloy capillary tubing; Seven, be annealing in process 2～8h under 200～420 ℃ of conditions with magnesium alloy capillary tubing in temperature, put into acetone-ethanol solution then and carry out ultrasonic processing 0.2～1.5h, be that 10%～20% glacial acetic acid aqueous solution is carried out pickling 10～60s with mass concentration more then, promptly get high-fineness ratio, magnesium alloy with high strength and ductility capillary; The internal diameter unanimity of cylinder tube in the diameter of dark consistent, the cylinder of cylinder tube and the step 3 in cylinder and the step 3 in the step 4 wherein; In the step 7 in acetone-ethanol solution acetone mix by 1: 1 volume ratio with absolute ethyl alcohol.
2. high-fineness ratio according to claim 1, magnesium alloy with high strength and ductility preparation method capillaceous is characterized in that magnesium alloy ingot is AZ31 magnesium alloy ingot or MB15 magnesium alloy ingot in the step 1.
3. high-fineness ratio according to claim 1 and 2, magnesium alloy with high strength and ductility preparation method capillaceous push under the condition that it is characterized in that in the step 1 being 10～45 in extrusion ratio, extrusion die drift speed is 22～28mm/s.
4. high-fineness ratio according to claim 3, magnesium alloy with high strength and ductility preparation method capillaceous is characterized in that in the step 2 in temperature being annealing in process 3～7h under 240～360 ℃ of conditions.
5. according to claim 1,2 or 4 described high-fineness ratios, magnesium alloy with high strength and ductility preparation method capillaceous, the tube base thickness degree that it is characterized in that cylinder in the step 3 is that the internal diameter of 2.5～4.5mm, the dark 12～20mm of being of tube, tube is Φ 13.7～Φ 13.8mm.
6. high-fineness ratio according to claim 5, magnesium alloy with high strength and ductility preparation method capillaceous is characterized in that the magnitude of interference is 0.03～0.07mm in the step 4.
7. according to claim 1,2,4 or 6 described high-fineness ratios, magnesium alloy with high strength and ductility preparation method capillaceous, push under the condition that it is characterized in that in the step 5 being 28～146, extrusion die drift speed is 22～28mm/s in extrusion ratio.
8. high-fineness ratio according to claim 7, magnesium alloy with high strength and ductility preparation method capillaceous is characterized in that the lengthening drill bit aperture is Φ 1.8～Φ 2.6mm in the step 6.
9. according to claim 1,2,4,6 or 8 described high-fineness ratios, magnesium alloy with high strength and ductility preparation method capillaceous, the mass concentration that it is characterized in that glacial acetic acid aqueous solution in the step 7 is 12%～18%.
10. high-fineness ratio according to claim 9, magnesium alloy with high strength and ductility preparation method capillaceous is characterized in that the pickling time is 20～50s in the step 7.
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| CN101829364B (en) * | 2010-06-22 | 2013-07-17 | 上海交通大学 | Method for preparing biodegradable magnesium alloy intravascular stent |
| CN102069103A (en) * | 2010-11-30 | 2011-05-25 | 于洋 | Plastic processing method for magnesium alloy capillary tube |
| CN102632183A (en) * | 2012-04-24 | 2012-08-15 | 江苏诚德钢管股份有限公司 | Production process of magnesium alloy medium-thick-wall tube with ultra-fine grain structure |
| CN103789711B (en) * | 2014-02-14 | 2016-03-16 | 西安爱德万思医疗科技有限公司 | A kind of preparation method of medical bio degradable zinc alloy capillary tubes |
| CN104947012B (en) * | 2015-07-08 | 2017-02-01 | 南昌航空大学 | Toughening method for novel temperature controller capillary material |
| CN105964716B (en) * | 2016-05-11 | 2020-10-16 | 郑州大学 | One-step forming processing method of magnesium alloy thin-walled capillary tube for intravascular stent |
| CN107838222B (en) * | 2016-09-18 | 2019-06-21 | 上海交通大学 | The preparation method and applications of biological medical degradable kirsite capillary tubes |
| CN109622660B (en) * | 2018-12-24 | 2021-05-11 | 有研工程技术研究院有限公司 | Preparation method of magnesium alloy precision pipe |
| CN113600728B (en) * | 2021-08-05 | 2022-11-29 | 沈阳工业大学 | High-precision magnesium alloy thin-wall micro-fine tube and composite preparation method thereof |
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