CN108213683A - A kind of preparation method of porous nickel titanium plate - Google Patents
A kind of preparation method of porous nickel titanium plate Download PDFInfo
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- CN108213683A CN108213683A CN201711472256.2A CN201711472256A CN108213683A CN 108213683 A CN108213683 A CN 108213683A CN 201711472256 A CN201711472256 A CN 201711472256A CN 108213683 A CN108213683 A CN 108213683A
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- porous nickel
- titanium plate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/001—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by extrusion or drawing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/023—Thermo-compression bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/22—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/24—Preliminary treatment
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Powder Metallurgy (AREA)
- Pressure Welding/Diffusion-Bonding (AREA)
Abstract
The present invention relates to a kind of preparation methods of porous nickel titanium plate, belong to technical field of metal material preparation.Preparation method disclosed by the invention is that the cold deformation NiTi net of clean surface is stacked, and using vacuum hot-pressing process, makes the atom phase counterdiffusion between NiTi contact surface, interpenetrates, be combined into an entirety, so as to obtain porous nickel titanium plate.The present invention can accelerate the speed and effect of Hot pressing diffusion using material of the cold deformation NiTi net of clean surface as vacuum hotpressing.The porous nickel titanium plate mesoporous gap that the present invention obtains is uniform, and population size is controllable, it is more advantageous to which objectionable impurities is few in porous nickel titanium plate, and grain structure is tiny, has excellent shape memory effect and super-elasticity, has very strong practicability.
Description
Technical field
The invention belongs to technical field of metal material preparation, more particularly to a kind of preparation method of porous nickel titanium plate.
Background technology
Nitinol is widely applied at present in biomedical materials field because of its unique excellent performance, including
Intervention support, correction silk and bone plate and bone nail etc..As Orthopedic medical metal material, the modular ratio of Nitinol
Common metal is much lower, only 80GPa or so, is a kind of good orthopedic implanting material, and body bone tissue elasticity modulus only has
20~40GPa, in contrast, the elasticity modulus of Nitinol is still higher.In addition the surface inertness of Nitinol makes it easily
It generates implantation and loosens failure.These problems all limit Nitinol further applying in field of orthopaedics.
In order to solve these problems, many researchers propose Nitinol being prepared into porous material, so as to obtain more
Excellent performance.Porous nickel-titanium alloy will have most rational combination in terms of intensity, rigidity and density, while porosity has
Conducive to growing into for induction bone tissue, the fixation for making implantation material is more safe and reliable.In addition more importantly porous nickel-titanium alloy
Shape memory effect and unique volume memory effect, make the implantation process of implantation material become simple, can mitigate patient's significantly
Pain.Porous nickel-titanium alloy will be as the hard tissue repairs such as bone, joint and tooth and the medical material of replacement, performance advantage
What other materials cannot compare.
But the preparation of porous nickel-titanium alloy is a difficult point.At present prepared by the most several porous alloys of domestic and international application
Method makes method, metaliding, infusion process, fibre metallurgy method and powder metallurgic method etc. including cast.Above method can be attributed to
Two classes, one kind are powder smelting to establish the modification method on the basis of the traditional method of smelting for preparing fine and close Nitinol, one kind
Golden and its derivative new method.Due to very active under titanium elements high temperature, it is various prepare porous nickel-titanium alloy method be difficult
The quantity of the impurity phases such as TiC, TiO2 is controlled, and TiNi2 difficult to control and TiNi3 etc. is without between the metal of shape memory effect
The formation of compound phase, porous nickel-titanium alloy prepared by these methods there are the problem of shape memory effect and poor super-elasticity,
So as to limit the application of porous nickel-titanium alloy.
Invention content
The object of the present invention is to provide a kind of porous nickel-titanium marmem preparation methods, solve current POROUS TITANIUM nickel and close
The problem of golden shape memory effect and poor super-elasticity.
It is another effective thinking to prepare porous nickel-titanium alloy by diffusion welding (DW) using block materials, but Nitinol
Diffusion Welding be a difficult point, the diffusion velocity of nickle atom and titanium atom differs greatly on one side weld interface, for a long time
Diffusion interfacial voids can be caused to influence welding effect instead；On the other hand tiny grain size is to the shape memory effect of alloy
It is of great significance with super-elasticity, excessive temperature is unfavorable to alloy property for a long time with crossing；How crystal grain tiny excellent is obtained
Matter weld interface is the problem that current Nitinol Pervasion Weld Technology needs solve.
To achieve the above object, the present invention takes following technical scheme：
After NiTi silk material is cold drawn to preliminary dimension and low temperature aligning, pickling removal surface oxide layer is prepared into plane titanium
Nickel wire net after surface active, multiple NiTi silk screens is stacked, and be put into the mold of vacuum hotpressing stove and be combined into
One entirety.
Another technical solution of the present invention is that the cold rolling nitinol sheet of clean surface is punching into NiTi net, by acid-wash activation
Afterwards, after same vacuum hot-pressing process, porous nickel titanium plate is formed.
Further, the vacuum hot-pressing process is：Vacuum degree is less than 10-2Pa, 800 DEG C~1000 DEG C of temperature, hot pressing pressure
0.5~5Mpa, 0.5~5h of hot pressing time.Make the atom phase counterdiffusion between titanium-nickel wire contact surface, interpenetrate, improve internal
Structure forms porous nickel-titanium alloy sheets.
Further, the titanium nickel screen is prepared using silk material weaving.
Further, the technological process of silk material braiding is：Nitinol alloy wire → drawing deformation → low temperature aligning → pickling
→ braiding silk screen → activation → stacking.
Further, the nitinol sheet passes through cold-rolling deformation → low temperature leveling → punching → pickling → activation → stacking → vacuum
Hot pressing → be shaped to porous nickel titanium plate.
Further, the drawing deformation or cold-rolling deformation, cold deformation are 30~50%.
Further, the low temperature aligning or low temperature leveling, temperature are 280-350 DEG C.
Further, the pickling is to carry out immersion 5min~1h using hydrochloric acid, then cleans surface with methanol, obtains activity
Then surface carries out vacuum hotpressing within 1h.
Further, the vacuum hot-pressing process, NiTi net is stacked and is put into vacuum hotpressing stove, alternating of often throwing the net
The 4mm that is all around staggered is placed.
The beneficial effects of the invention are as follows：
1st, the present invention prepares porous nickel titanium plate using block materials, does not introduce additive, and being avoided that in preparation process can shape
Into the impurity phases such as other intermetallic compounds such as TiNi2 and TiNi3 and TiC, TiO2, so as to retain its good shape memory
Effect and super-elasticity；
2nd, the present invention carries out vacuum hotpressing diffusion welding (DW) using NiTi cold deformation material, and the cold deformed microstructure of Nitinol is in height
During the lower progress recovery and recrystallization of temperature, larger change in shape will be generated, on the one hand can crush the oxide layer of contact surface,
On the other hand it can increase the contact of contact surface, therefore relatively low temperature, relatively low pressure and shorter may be used
Time completes Diffusion Welding, and the crystal grain of alloy can still retain smaller form, so as to obtain good shape memory effect and
Hyperelastic porous nickel titanium plate.
3rd, the present invention can reduce Nitinol surface oxide layer thickness, and in material table using hydrochloric acid as activator
Face forms the etch pit of small non-oxidation layer, can reduce the diffusional resistance of titanium atom in this way, can equally reach quickening and expand
Dissipate the effect of speed of welding.It is cleaned using methanol and is to be formed newly on NiTi surface without the purpose of other solvents cleaning
Oxide layer.
4th, the present invention is by adjusting silk material diameter and silk screen pore-size, can obtain the more of Different porosities and pore size
Porous materials, it is applied widely.
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is further described, following embodiment is only used for more
Add and clearly demonstrate technical scheme of the present invention, do not limited the scope of the invention with this.
Embodiment 1
A kind of technical solution that porous nickel titanium plate is prepared using titanium-nickel wire：
The first step using the titanium-nickel wire of Φ 0.13mm, is cold drawn to 0.1mm, cold deformation 41% after annealing.
0.1mm titanium-nickel wires are carried out low temperature straightening processing by second step by 300 DEG C of tube furnace.
Third walks, the surface casting skin of pickling titanium-nickel wire.
4th step：0.1mm titanium-nickel wires are woven into grid 1mm*1mm, the NiTi net of length and width size 200mm*200mm.
5th step：Immersion 30min is carried out using hydrochloric acid, is then cleaned up with methanol.
6th step：50 NiTi nets are stacked and are put into vacuum hotpressing stove.
7th step：Hot pressing parameters are less than 10 for vacuum degree-2Pa, 950 DEG C of temperature, pressure 1Mpa, time 1h.
8th step：After being cooled to room temperature, porous nickel titanium plate is taken out.
It is about 3mm that thickness, which can be obtained, and the porous nickel titanium plate of length and width 200mm*200mm, porosity is about 70~80%.
Embodiment 2
A kind of technical solution that porous nickel titanium plate is prepared using nitinol sheet：
The first step using the nitinol sheet of Φ 0.45mm, is cold-rolled to 0.3mm, cold deformation 33% after annealing.
0.3mm nitinol sheets are carried out low temperature leveling processing by second step by 300 DEG C of batch-type furnace.
Third walks, and nitinol sheet is punching into size of mesh opening 8mm*8mm, quantity 20*20, length and width size 200mm*200mm's
NiTi net.
4th step：The surface oil pollution layer of pickling nitinol sheet.
5th step：Immersion 30min is carried out using hydrochloric acid, is then cleaned up with methanol.
6th step：50 NiTi nets are stacked and are put into vacuum hotpressing stove, often throws the net and is alternately all around staggered
4mm is placed.
7th step：Hot pressing parameters are less than 10 for vacuum degree-2Pa, 950 DEG C of temperature, pressure 1Mpa, time 1h.
8th step：After being cooled to room temperature, porous nickel titanium plate is taken out.
It is about 12mm that thickness, which can be obtained, the porous nickel titanium plate of length and width 200mm*200mm, and porosity is about 40~
50%.
The above is only the more excellent embodiment of the present invention, non-that the present invention is imposed any restrictions, every according to the present invention
Technical spirit still falls within technical solution of the present invention to implementing any simple modification, change and the equivalent transformation that are made above
Protection domain in.
Claims (10)
1. a kind of preparation method of porous nickel titanium plate, which is characterized in that using vacuum hot-pressing process, the titanium nickel screen of stacking is combined
Into an entirety, make the atom phase counterdiffusion between NiTi contact surface, interpenetrate, so as to obtain porous nickel titanium plate.
2. preparation method according to claim 1, which is characterized in that the titanium nickel screen is prepared using silk material weaving
's.
3. preparation method according to claim 1, which is characterized in that the titanium nickel screen is that nitinol sheet is punching into NiTi
Net is formed after acid-wash activation.
4. preparation method according to claim 1, which is characterized in that the vacuum hot-pressing process is：Vacuum degree is less than 10- 2Pa, 800 DEG C~1000 DEG C of temperature, 0.5~5Mpa of hot pressing pressure, 0.5~5h of hot pressing time.
5. preparation method according to claim 2, which is characterized in that the technological process of silk material braiding is：NiTi closes
Spun gold → drawing deformation → low temperature aligning → pickling → braiding silk screen → activation → stacking.
6. preparation method according to claim 3, which is characterized in that the nitinol sheet passes through cold-rolling deformation → low temperature leveling
→ punching → pickling → activation → stacking → vacuum hotpressing → is shaped to porous nickel titanium plate.
7. preparation method according to claim 5 or 6, which is characterized in that the drawing deformation or cold-rolling deformation, cold change
Shape amount is 30~50%.
8. preparation method according to claim 5 or 6, which is characterized in that the low temperature aligning or low temperature leveling, temperature are
280-350℃。
9. preparation method according to claim 5 or 6, which is characterized in that the pickling is impregnated using hydrochloric acid
Then 5min~1h cleans surface with methanol, obtain active surface, vacuum hotpressing is then carried out within 1h.
10. preparation method according to claim 1, which is characterized in that NiTi net is stacked on by the vacuum hot-pressing process
It is put into togerther in vacuum hotpressing stove, the 4mm placements that are alternately all around staggered of often throwing the net.
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| CN201711472256.2A CN108213683A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation method of porous nickel titanium plate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110560695A (en) * | 2019-09-03 | 2019-12-13 | 西安建筑科技大学 | Titanium-based functional gradient material with porous surface and preparation method thereof |
| CN111014335A (en) * | 2019-12-24 | 2020-04-17 | 武汉理工大学 | Porous metal material and preparation method thereof |
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| JPS5656795A (en) * | 1979-09-28 | 1981-05-18 | Leuven Res & Dev Vzw | Composite material for prosthetic |
| CN1070230A (en) * | 1991-09-06 | 1993-03-24 | 中国科学院金属研究所 | The reparation technology of a kind of titanium-nickel alloy foil and sheet material |
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| CN103060590A (en) * | 2013-01-08 | 2013-04-24 | 西北工业大学 | Preparation method of gradient porous titanium alloy |
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2017
- 2017-12-29 CN CN201711472256.2A patent/CN108213683A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5656795A (en) * | 1979-09-28 | 1981-05-18 | Leuven Res & Dev Vzw | Composite material for prosthetic |
| CN1070230A (en) * | 1991-09-06 | 1993-03-24 | 中国科学院金属研究所 | The reparation technology of a kind of titanium-nickel alloy foil and sheet material |
| CN101011874A (en) * | 2007-01-22 | 2007-08-08 | 浙江大学 | Lightening fire resistant polymer porous membrane laminated composite material and manufacturing method thereof |
| CN103060590A (en) * | 2013-01-08 | 2013-04-24 | 西北工业大学 | Preparation method of gradient porous titanium alloy |
| CN103317225A (en) * | 2013-05-28 | 2013-09-25 | 西北工业大学 | Vacuum diffusion bonding method for TC18 titanium alloys |
| CN103401003A (en) * | 2013-07-17 | 2013-11-20 | 南京大学昆山创新研究院 | Gas diffusion layer of PEMFC (Proton Exchange Membrane Fuel Cell) and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110560695A (en) * | 2019-09-03 | 2019-12-13 | 西安建筑科技大学 | Titanium-based functional gradient material with porous surface and preparation method thereof |
| CN111014335A (en) * | 2019-12-24 | 2020-04-17 | 武汉理工大学 | Porous metal material and preparation method thereof |
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