CN106222467A - A kind of titanium material with high-orientation stratiform orientation interconnected pore and preparation method thereof - Google Patents
A kind of titanium material with high-orientation stratiform orientation interconnected pore and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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- 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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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- 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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- C22C14/00—Alloys based on titanium
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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Abstract
The present invention relates to a kind of titanium material with high-orientation stratiform orientation interconnected pore and preparation method thereof.Belong to porous metal material preparing technical field.Titanium material designed by the present invention has highly directional layered poros and layer is connected by bracing frame with layer.The aperture of described highly directional layered poros is 1.2 8.3cm, and interlamellar spacing is 5～180 μm.The present invention is by being placed with the insulator at certain angle of inclination in a mold, titaniferous water-based slurry is injected in mould, the Double-direction Temperature field utilizing design makes slurry directional solidification molding, ice crystal is removed in gained cold base lyophilization, low temperature removing binding agent, sintered at high temperature titanium or titanium alloy porous material.By controlling solid concentration, the angle of inclination of insulator and freezing conditions in slurry, the porous titanium or titanium alloy porous material of highly directional, large aperture and high porosity can be obtained.It is simple that the present invention has technique, is suitable for preparation and has high porosity and highly directional layered poros material.
Description
Technical field
The present invention relates to a kind of titanium material with high-orientation stratiform orientation interconnected pore and preparation method thereof.Belong to porous
Technical field of metal material preparation.
Background technology
Porous titanium or titanium alloy has the physical chemistry such as the corrosion resistance of excellence, high specific strength, good biocompatibility
The functional characteristics such as the permeability that performance and low density, big specific surface area are become reconciled, are filtering separation, air-breathing sound absorption, energy suction
The fields such as receipts, electrode, bio-medical are increasingly widely applied.In recent years, porous titanium or titanium alloy is often by as bone group
Knit implantation and dental restoration material and studied widely.And the form of porous titanium or titanium alloy mesopore, aperture, porosity, company
The structural characteristic parameters such as the general character are most important to the growth of osseous tissue.
Preparation porous titanium or titanium alloy most common method has powder metallurgic method, slurry foaming, ice template method at present, its
Middle powder metallurgic method is by adding in titanium or titanium alloy powder by pore creating material such as carbamide, ammonium hydrogen carbonate, starch, by mixing,
The technique removing pore creating materials such as compacting, sintering, powder particle sintering prepares titanium or titanium alloy porous material.This method is prepared many
Hole titanium or titanium alloy porosity is relatively low, and the aperture of material is difficult to accurately control.Slurry foaming it is critical only that control slurry
Viscosity and the size of bubble, but generally the size of bubble and the distribution mode of bubble are the most rambunctious, and this also results in
Use the pore size of material prepared by the method uneven.Ice template method is to be oriented slurry under certain temperature field
Cryocoagulation, makes powder particle carry out assembling weight during the oriented growth of ice crystal under the pushing repulsive force effect of ice crystal
Row, gained ice base processes through vacuum lyophilization, finally leaves the porous laminated structure that having with ice as template aligns.
Laminar hole structure prepared by this method, has the feature of high porosity and intercommunicating pore, it is easy to bone growth.Additionally, obtain many
Porous materials hole is interconnected, and has good permeability.Heavier yet with metal dust, it is hardly formed uniform and stable slurry
Material, the porous material synthesized by this method at present mostly is ceramic material.Recently, researcher is also attempted preparing POROUS TITANIUM by this method.But
Report all uses alkene as solvent, and alkene icing rate is relatively slow, is hardly formed longer ice crystal, therefore is difficult to acquisition and has stratiform
The POROUS TITANIUM of structure.As [Acta Biomaterialia, 2012,8,2401-2410] such as Yook takes reverse temperature field to make ice
Crystalline substance grows from top to bottom, has prepared a kind of POROUS TITANIUM with new structure, but layer structure in POROUS TITANIUM inconspicuous.
Additionally, use the virose organic solvent camphene of tool to prepare slurry, operating process can be made troubles, and environment can be caused dirt simultaneously
Dye.
Summary of the invention
It is an object of the invention to provide a kind of titanium material with high-orientation stratiform orientation interconnected pore and preparation method thereof.
A kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention；Described titanium material has highly directional stratiform hole
Gap and layer are connected by bracing frame with layer.
A kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention；The aperture of described highly directional layered poros
For 1.2-8.3cm, being preferably 2.1-5.2cm, more preferably 2.3-4.0cm, interlamellar spacing is 5～180 μm.
A kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention；The orientation of described highly directional layered poros
Degree is more than or equal to 90%.The perforate direction that the degree of orientation is oriented laminated hole of the most described highly directional layered poros
Concordance, its expression formula can be: the oriented laminated number of pores in same perforate direction in the degree of orientation of oriented laminated hole=titanium material
The total number of oriented laminated hole in mesh/titanium material.
A kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention；Described aperture is approximate aperture, i.e. hole
Cross-sectional area be converted into circle, this circle corresponding to diameter.
A kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention；On described casing play and/or bracing frame
Aperture is also distributed.
A kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention；The porosity of described porous body be 30～
90%, it is preferably 50%-85%, more preferably 70%-85%.
A kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention；The material of described titanium material is pure titanium or titanium
Alloy.In described titanium alloy, the weight/mass percentage composition of titanium elements is more than or equal to 50%.
The preparation method of a kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention, comprises the steps:
(1) metal dust is mixed homogeneously with water mixed liquid 2:98～60:40 by volume, obtain water-based slurry；Described
Containing binding agent in mixed liquor, and 1%～5% that the quality of binding agent is water quality, preferably 1～4%, more preferably
1.5%～3%.
(2) water-based slurry injection is placed with in the insulator mould with angle of inclination, in the Double-direction Temperature gradient of design
Low temperature solidification in Chang, puts into after slurry completely freezing and is vacuum dried 30～50h in freeze drying box；In described orientation temperature field
Bottom temp is less than head temperature, and described bottom temp is-5 DEG C～-100 DEG C, and preferably-20～-70 DEG C, head temperature is less than
Equal to 5 DEG C, and the temperature difference of bottom temp and head temperature is more than or equal to 20 DEG C；
(3) base substrate after lyophilization is removed from the molds, in vacuum or argon gas atmosphere, with the speed of 5～10 DEG C/min
Rate is heated to 300～550 DEG C, preferably 350～500 DEG C, more preferably 380～450 DEG C, is incubated removing in 1～3 hour and adds
The binding agent added；Rise to 1100～1250 DEG C with the speed of 5～10 DEG C/min further, preferably 1150～1200 DEG C, be incubated 2
～4h.Furnace cooling, to room temperature, obtains the titanium material with high-orientation stratiform orientation interconnected pore.
The preparation method of a kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention, described metal dust
Granularity is 0.3 μm～5.0 μm.
The preparation method of a kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention, metal dust is titanium
At least one in powder, hydride powder, titanium and other metal dust mixed powder, Titanium Powder.As: aluminium during preparation TC4
Powder, admire powder, vanadium powder, and described powder size are 0.3～5.0 μm.
The preparation method of a kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention, described binding agent is selected from
At least one in gelatin, polyvinyl alcohol, chitosan, polyacrylic acid, preferably gelatin.
The preparation method of a kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention, described insulator poly-two
One in methylsiloxane, polyethylene, epoxy resin, preferably polydimethylsiloxane.
The preparation method of a kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention, inclining of described insulator
Oblique angle excursion between 5～25 °, preferably 10～20 °.
The preparation method of a kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention, described inclination angle is exhausted
The angle that the inclined plane of hot body and bottom surface copper coin are formed.Described bottom surface copper coin is the bottom surface copper base of refrigerating plant.
Preferably, the preparation method of a kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention,
Metal dust 50g is mixed with water night (aqueous 60g, gelatin 1.2g) mix homogeneously and obtains water-based slurry；Or
Metal dust 52g is mixed with water night (aqueous 70g, gelatin 2.1) mix homogeneously and obtains water-based slurry；Or
Metal dust 50g is mixed with water night (aqueous 355g, polyvinyl alcohol 6.7g) mix homogeneously and obtains water-based slurry.
The present invention is a kind of has a titanium material of high-orientation stratiform orientation interconnected pore and osseous tissue has and is similarly directed hole
Structure, can be applied to the medical domains such as Bone Defect Repari as osseous tissue substitution material.
A kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention, has good permeability, can conduct
Filtering material is applied to filter separation field.
A kind of titanium material with high-orientation stratiform orientation interconnected pore of the present invention, after supported catalyst, can be used for industry
The fields such as catalysis.
Principle and advantage
The present invention, by putting into insulator, defines the temperature field of both direction, has obtained having high-orientation stratiform fixed
To the titanium or titanium alloy porous material in hole.
The present invention is by the particle diameter of material powder, consumption, and bonding agent kind is especially with gelatin, freezing conditions (temperature
Field, cooldown rate, insulator inclination angle) synergism, the porosity of titanium or titanium alloy porous material, aperture and micro-can be realized
The finely regulating of structure.
Accompanying drawing explanation
Accompanying drawing 1 is the refrigerating plant schematic diagram being placed with insulator mould
Accompanying drawing 2 is the cross-sectional scans Electronic Speculum figure of the POROUS TITANIUM with highly directional hole of the embodiment of the present invention 1；
The relative position relation of the angle of inclination of insulator and insulator and bottom surface copper coin is can be seen that from accompanying drawing 1.
Wherein accompanying drawing 2 (a) is the Electronic Speculum figure of 200 times, and accompanying drawing 2 (b) is the Electronic Speculum figure of 2000 times；As seen in Figure 2
Prepared POROUS TITANIUM has the pore structure of oriented laminated distribution.
Fig. 3 is 200 times of Electronic Speculum figures of POROUS TITANIUM prepared by comparative example, it can be seen that the hole of POROUS TITANIUM is along different directions, no
There is high-orientation.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
50g titanium valve is added, the mixed liquor ball milling mixing of 60g deionized water and 1.2g gelatin (binding agent) in ball grinder
After 12h, obtain uniform water base titanium slurry；Water-based slurry is injected and is placed with the insulator (inclination angle is 15 °) with inclination angle
In mould (square plastic mould), then mould is put into lower end and connects on the copper base of refrigerating plant, awkward silence at a meeting lower end temperature is set
Spend-30 DEG C, upper end temperature 5 DEG C, move on to freezer dryer is removed ice crystal after base substrate freezing completely.After drying, base substrate is shifted
Sinter in vacuum drying oven, be heated to 400 DEG C with the speed of 3 DEG C/min and be incubated 2 hours, the binding agent that removing is added；Further with 5
DEG C/speed of min rises to 1200 DEG C of insulation 3h, takes out sample after furnace temperature is as cold as room temperature.Obtaining porosity is 70%, directional hole
Interlamellar spacing is～the POROUS TITANIUM of 25 μm.In sample, the aperture of highly directional layered poros is 1.3-3.0cm, described highly directional stratiform hole
The degree of orientation of gap is more than or equal to 90%.
Embodiment 2:
The mixed of 45g titanium valve, 3g aluminium powder, 4g vanadium powder, 70g deionized water and 2.1g gelatin (binding agent) is added in ball grinder
After closing liquid ball milling mixing 24h, obtain uniform water base mixed powder slurry；Inject water-based slurry to be placed with and there is inclination angle (inclination
Angle is 10 °) insulator mould in (square plastic mould), then mould is put into lower end connect refrigerating plant copper base
On, awkward silence at a meeting lower temperature-20 DEG C, upper end temperature 0 DEG C are set, after base substrate freezing completely, move on to freezer dryer is removed ice crystal.
After drying, transferring to base substrate sinter in vacuum drying oven, be heated to 350 DEG C of insulation 2h with the speed of 5 DEG C/min, it is viscous that removing is added
Knot agent；Rise to 1250 DEG C of insulation 2h with the speed of 8 DEG C/min further, after furnace temperature is as cold as room temperature, takes out sample.Obtain hole
Rate is 60%, and directional hole interlayer aperture is～porous Ti-6Al-4V (TC4) alloy of 40 μm.The hole of sample orientation layered poros
Footpath is 1.2-2.5cm, and the degree of orientation of described highly directional layered poros is more than or equal to 90%.
Embodiment 3:
50g titanium valve, 335g deionized water and the mixed liquor ball milling of 6.7g polyvinyl alcohol (binding agent) is added in ball grinder
After mixing 18h, obtain uniform water base titanium slurry；Inject water-based slurry to be placed with and there is the insulator at inclination angle (inclination angle is
25 °) in mould (square plastic mould), then mould is put into lower end and connects on the copper base of refrigerating plant, arrange under awkward silence at a meeting
End temperature-50 DEG C, upper end temperature-5 DEG C, after base substrate is freezing completely, move on to freezer dryer is removed ice crystal.After drying, will
Base substrate is transferred to sinter in argon gas atmosphere, is heated to 350 DEG C with the speed of 5 DEG C/min and is incubated 3 hours, the bonding that removing is added
Agent；Rise to 1200 DEG C of insulation 2h with the speed of 5 DEG C/min further, after furnace temperature is as cold as room temperature, takes out sample.Obtain porosity
Being 87%, interlayer aperture is～the POROUS TITANIUM of 180 μm.In sample, the aperture of highly directional layered poros is 2.8-7.5cm, described height
The degree of orientation of oriented laminated hole is more than or equal to 90%.
Comparative example
Do not put insulator
50gTi powder is added, the mixed liquor ball milling mixing of 70g deionized water and 2.1g gelatin (binding agent) in ball grinder
After 24h, obtain uniform water base mixed powder slurry；Water-based slurry is injected in mould, then mould is put into lower end and connects cold
Freeze on the copper base of device, awkward silence at a meeting lower temperature-20 DEG C, upper end temperature 0 DEG C are set, after base substrate freezing completely, move on to lyophilization
Machine is removed ice crystal.After drying, transfer to base substrate vacuum drying oven sinters, be heated to 350 DEG C of insulations with the speed of 5 DEG C/min
2h, the binding agent that removing is added；Rise to 1250 DEG C of insulation 2h with the speed of 8 DEG C/min further, take after furnace temperature is as cold as room temperature
Go out sample.Obtaining porosity is 62%, and directional hole interlayer aperture is～porous Ti of 40 μm.Sample laminate hole is along not Tongfang
To, not there is high-orientation.
Claims (10)
1. a titanium material with high-orientation stratiform orientation interconnected pore；It is characterized in that: described titanium material has highly directional layer
Shape hole and layer are connected by bracing frame with layer.
A kind of titanium material with high-orientation stratiform orientation interconnected pore the most according to claim 1；It is characterized in that: institute
The aperture stating highly directional layered poros is 1.2-8.3cm, and interlamellar spacing is 5～180 μm.
A kind of titanium material with high-orientation stratiform orientation interconnected pore the most according to claim 1；It is characterized in that: institute
State the degree of orientation of highly directional layered poros more than or equal to 90%.
A kind of titanium material with high-orientation stratiform orientation interconnected pore the most according to claim 1；It is characterized in that: institute
State and aperture on casing play and/or bracing frame, is also distributed.
A kind of titanium material with high-orientation stratiform orientation interconnected pore the most according to claim 1；It is characterized in that: institute
The porosity stating porous body is 30～90%.
6. prepare the side as described in claim 15 any one with high-orientation stratiform orientation interconnected pore titanium material for one kind
Method, it is characterised in that comprise the steps:
(1) metal dust is mixed homogeneously with water mixed liquid 2:98～60:40 by volume, obtain water-based slurry；Described mixing
Containing binding agent in liquid, and 1%～5% that the quality of binding agent is water quality；
(2) water-based slurry injection is placed with in the insulator mould with inclination angle, low in the Double-direction Temperature gradient fields of design
Temperature solidification, puts into after slurry completely freezing and is vacuum dried 30～50h in freeze drying box；Bottom temperature in described orientation temperature field
Degree is less than head temperature, and described bottom temp is-5 DEG C～-100 DEG C, and the temperature difference of bottom temp and head temperature is more than or equal to
20℃；
(3) base substrate after lyophilization is removed from the molds, in vacuum or argon gas atmosphere, adds with the speed of 5～10 DEG C/min
Heat, to 300～550 DEG C, is incubated 1～3 hour；Then rise to 1100～1250 DEG C with the speed of 5～10 DEG C/min, insulation 2～
4h；Furnace cooling, to room temperature, obtains the titanium material with high-orientation stratiform orientation interconnected pore.
The preparation method of a kind of titanium material with high-orientation stratiform orientation interconnected pore the most according to claim 6, its
It is characterised by: the granularity of described metal dust is 0.3 μm～5.0 μm.
A kind of preparation method with high-orientation stratiform orientation interconnected pore titanium material the most according to claim 6, it is special
Levy and be:
At least one in gelatin, polyvinyl alcohol, chitosan, polyacrylic acid of described binding agent；
The material of described insulator mould one in polydimethylsiloxane, polyethylene, epoxy resin；
The angle change scope of described insulator is between 5～25 °.
9., according to a kind of titanium material with high-orientation stratiform orientation interconnected pore of claim 1-5 any one gained, it is special
Levy and be: described titanium material is used as osseous tissue substitution material and is applied to the medical domains such as Bone Defect Repari.
10., according to a kind of titanium material with high-orientation stratiform orientation interconnected pore of claim 1-5 any one gained, it is special
Levy and be: described titanium material is applied to filter separation field as filtering material；Or
After described titanium material supported catalyst, for Industrial Catalysis field.
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| CN107746985A (en) * | 2017-10-09 | 2018-03-02 | 常州禾吉纺织品有限公司 | A kind of preparation method of stratiform interworking architecture composite |
| CN108437154A (en) * | 2018-04-16 | 2018-08-24 | 西安建筑科技大学 | Freezing casting prepares the mold that uniform orientation freezing can be achieved in porous ceramics technique |
| CN110280766B (en) * | 2019-07-23 | 2020-08-04 | 中南大学 | Hierarchical pore structure nickel-based alloy and preparation method and application thereof |
| CN110280766A (en) * | 2019-07-23 | 2019-09-27 | 中南大学 | Hierarchical porous structure nickel-base alloy and its preparation method and application |
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| CN110732672A (en) * | 2019-12-11 | 2020-01-31 | 中南大学 | gradient metal-based porous material and preparation method and application thereof |
| CN110732672B (en) * | 2019-12-11 | 2022-05-03 | 中南大学 | Gradient metal-based porous material and preparation method and application thereof |
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| CN112548100A (en) * | 2020-12-24 | 2021-03-26 | 南京航空航天大学 | Preparation method of bionic oriented ordered laminated composite material |
| CN113956063A (en) * | 2021-10-26 | 2022-01-21 | 浙江大学 | Preparation method of porous material with long-range oriented structure or complex structure |
| CN113956063B (en) * | 2021-10-26 | 2022-09-20 | 浙江大学 | Preparation method of porous material with long-range oriented structure or complex structure |
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