CN106222467B - A kind of titanium with high-orientation stratiform orientation interconnected pore and preparation method thereof - Google Patents
A kind of titanium 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
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
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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
- A61L27/02—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
- A61L27/56—Porous materials, e.g. foams or sponges
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- 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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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Abstract
The present invention relates to a kind of titanium with high-orientation stratiform orientation interconnected pore and preparation method thereof.Belong to porous metal material preparing technical field.Titanium designed by the present invention has highly directional layered poros and layer is connected with layer by support frame.The aperture of the highly directional layered poros is 1.2 8.3cm, and interlamellar spacing is 5~180 μm.Heat guard of the invention by being put into certain angle of inclination in a mold, titaniferous water-based slurry is injected in mould, slurry directional solidification is molded using the Double-direction Temperature field of design, the cold base freeze-drying of gained removes ice crystal, low temperature removes binding agent, sintered at high temperature titanium or titanium alloy porous material.By controlling solid concentration in slurry, the angle of inclination of heat guard and freezing conditions, the porous titanium or titanium alloy porous material of highly directional, large aperture and high porosity can be obtained.The present invention has technique simple, and being suitable for preparing has high porosity and highly directional layered poros material.
Description
Technical field
The present invention relates to a kind of titanium 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 excellent corrosion resistance, high specific strength, good biocompatibility
The functional characteristics such as the permeability that performance and low density, big specific surface area are become reconciled, be separated by filtration, air-breathing sound absorption, energy inhale
The fields such as receipts, electrode, bio-medical obtain more and more extensive application.In recent years, porous titanium or titanium alloy is often by as bone group
Knit implantation and dental restoration material and widely studied.And the form of porous titanium or titanium alloy mesopore, aperture, porosity, company
Growth of the structural characteristic parameters such as the general character to bone tissue is most important.
Preparing the most frequently used method of porous titanium or titanium alloy at present has powder metallurgic method, slurry foaming, ice template method, its
Middle powder metallurgic method be by the way that pore creating material such as urea, ammonium hydrogen carbonate, starch are added in titanium or titanium alloy powder, by mixing,
The technique removing pore creating material such as compacting, sintering, powder particle sintering prepare titanium or titanium alloy porous material.This method is prepared more
Hole titanium or titanium alloy porosity is relatively low, and the aperture of material is difficult accurately to control.The key of slurry foaming is to control slurry
Viscosity and bubble size, but the generally size of bubble and the distribution mode of bubble is very rambunctious, and this is also resulted in
Pore size using material prepared by this method is uneven.Ice template method is that slurry is oriented under certain temperature field
Cryocoagulation, make to carry out aggregation weight under pushing repulsive force effect of the powder particle in ice crystal during the oriented growth of ice crystal
Row, gained ice base handles through vacuum freeze drying, and it is template with the porous laminated structure aligned finally to leave using ice.
Laminar hole structure prepared by this method, there is the feature of high porosity and intercommunicating pore, be easy to bone growth.In addition, what is obtained is more
Porous materials hole is interconnected, and has good permeability.It is heavier yet with metal dust, it is hardly formed uniform and stable slurry
Material, the porous material synthesized at present with this method is mostly ceramic material.Recently, researcher also attempts to prepare POROUS TITANIUM with this method.But
For report all using down alkene as solvent, down alkene icing rate is slower, is hardly formed longer ice crystal, therefore is difficult to obtain to have stratiform
The POROUS TITANIUM of structure.Such as Yook [Acta Biomaterialia, 2012,8,2401-2410] 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 the layer structure in POROUS TITANIUM and unobvious.
In addition, preparing slurry using having virose organic solvent amphene, operating process can make troubles, while can cause dirt to environment
Dye.
The content of the invention
It is an object of the invention to provide a kind of titanium with high-orientation stratiform orientation interconnected pore and preparation method thereof.
A kind of titanium with high-orientation stratiform orientation interconnected pore of the present invention；The titanium has highly directional stratiform hole
Gap and layer is connected with layer by support frame.
A kind of titanium with high-orientation stratiform orientation interconnected pore of the present invention；The aperture of the highly directional layered poros
For 1.2-8.3cm, preferably 2.1-5.2cm, more preferably 2.3-4.0cm, interlamellar spacing is 5~180 μm.
A kind of titanium with high-orientation stratiform orientation interconnected pore of the present invention；The orientation of the highly directional layered poros
Degree is more than or equal to 90%.The degree of orientation of highly directional layered poros described in the present invention is the opening direction of oriented laminated hole
Uniformity, its expression formula can be：The oriented laminated number of pores of same opening direction in the degree of orientation=titanium of oriented laminated hole
The total number of oriented laminated hole in mesh/titanium.
A kind of titanium with high-orientation stratiform orientation interconnected pore of the present invention；The aperture is approximate aperture, i.e. hole
Cross-sectional area be converted into circle, the diameter corresponding to the circle.
A kind of titanium with high-orientation stratiform orientation interconnected pore of the present invention；On the casing play and/or support frame
Aperture is also distributed with.
A kind of titanium with high-orientation stratiform orientation interconnected pore of the present invention；The porosity of the porous body be 30~
90%th, it is preferably 50%-85%, more preferably 70%-85%.
A kind of titanium with high-orientation stratiform orientation interconnected pore of the present invention；The material of the titanium is pure titanium or titanium
Alloy.The weight/mass percentage composition of titanium elements is more than or equal to 50% in the titanium alloy.
A kind of preparation method of the titanium with high-orientation stratiform orientation interconnected pore of the present invention, comprises the steps：
(1) by metal dust and water mixed liquid by volume 2：98~60：40 is well mixed, obtains water-based slurry；It is described
Contain binding agent in mixed liquor, and the quality of binding agent is the 1%~5%, preferably 1~4% of water quality, more preferably
1.5%~3%.
(2) water-based slurry injection is placed with the adiabatic mould with angle of inclination, in the Double-direction Temperature gradient of design
Low temperature is solidified in, and 30~50h of vacuum drying in freeze drying box is put into after slurry completely freezing；In the orientation temperature field
Bottom temp is less than head temperature, and the bottom temp is -5 DEG C~-100 DEG C, is 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 freeze-drying is removed from the molds, in vacuum or argon gas atmosphere, with 5~10 DEG C/min speed
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；1100~1250 DEG C, preferably 1150~1200 DEG C, insulation 2 are further risen to 5~10 DEG C/min speed
~4h.Furnace cooling obtains the titanium with high-orientation stratiform orientation interconnected pore to room temperature.
A kind of preparation method of the titanium with high-orientation stratiform orientation interconnected pore of the present invention, the metal dust
Granularity is 0.3 μm~5.0 μm.
A kind of preparation method of the titanium with high-orientation stratiform orientation interconnected pore of the present invention, metal dust is titanium
At least one of powder, hydride powder, titanium and other metal dust mixed powders, Titanium Powder.Such as:Prepare TC4 when from aluminium powder,
Powder, vanadium powder by the emperor himself, and the powder size is 0.3~5.0 μm.
A kind of preparation method of the titanium with high-orientation stratiform orientation interconnected pore of the present invention, the binding agent are selected from
At least one of gelatin, polyvinyl alcohol, chitosan, polyacrylic acid, preferably gelatin.
A kind of preparation method of the titanium with high-orientation stratiform orientation interconnected pore of the present invention, the heat guard poly- two
One kind in methylsiloxane, polyethylene, epoxy resin, preferably dimethyl silicone polymer.
A kind of preparation method of the titanium with high-orientation stratiform orientation interconnected pore of the present invention, the heat guard are inclined
Oblique angle excursion is between 5~25 °, preferably 10~20 °.
A kind of preparation method of the titanium with high-orientation stratiform orientation interconnected pore of the present invention, the inclination angle is exhausted
The angle that the inclined plane of hot body is formed with bottom surface copper coin.The bottom surface copper coin is the bottom surface copper base of refrigerating plant.
Preferably, a kind of preparation method of the titanium with high-orientation stratiform orientation interconnected pore of the present invention,
Metal dust 50g mixes with water to night (aqueous 60g, gelatin 1.2g) well mixed obtains water-based slurry；Or
Metal dust 52g mixes with water to night (aqueous 70g, gelatin 2.1) well mixed obtains water-based slurry；Or
Metal dust 50g mixes with water to night (aqueous 355g, polyvinyl alcohol 6.7g) well mixed obtains water-based slurry.
The present invention it is a kind of with high-orientation stratiform orient interconnected pore titanium and bone tissue with being similarly directed hole
Structure, bone tissue alternative materials can be used as to be applied to the medical domains such as Bone Defect Repari.
A kind of titanium with high-orientation stratiform orientation interconnected pore of the present invention, has good permeability, can conduct
Filtering material is applied to be separated by filtration field.
A kind of titanium with high-orientation stratiform orientation interconnected pore of the present invention, after supported catalyst, available for industry
The fields such as catalysis.
Principle and advantage
The present invention forms the temperature field of both direction, has obtained that there is high-orientation stratiform to determine by being put into insulator
To the titanium or titanium alloy porous material in hole.
Particle diameter of the present invention by material powder, dosage, bonding agent species is especially with gelatin, freezing conditions (temperature
Field, cooldown rate, heat guard inclination angle) synergy, the porosity of titanium or titanium alloy porous material, aperture and micro- can be achieved
The finely regulating of structure.
Brief description of the drawings
Accompanying drawing 1 is the refrigerating plant schematic diagram for being placed with adiabatic mould
Accompanying drawing 2 is the cross-sectional scans electron microscope of the POROUS TITANIUM with highly directional hole of the embodiment of the present invention 1；
It can be seen that the angle of inclination of heat guard and heat guard and the relative position relation of bottom surface copper coin from accompanying drawing 1.
Wherein accompanying drawing 2 (a) is 200 times of electron microscope, and accompanying drawing 2 (b) is 2000 times of electron microscope；As seen in Figure 2
Prepared POROUS TITANIUM has the pore structure of oriented laminated distribution.
Fig. 3 is 200 times of electron microscopes of POROUS TITANIUM prepared by comparative example, it can be seen that the hole of POROUS TITANIUM is along different directions, no
With high-orientation.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1：
The mixed liquor ball milling mixing of 50g titanium valves, 60g deionized waters and 1.2g gelatin (binding agent) is added into ball grinder
After 12h, uniform water base titanium slurry is obtained；Water-based slurry injection is placed with to the heat guard with inclination angle (inclination angle is 15 °)
In mould (square plastic mould), then mould is put on the copper base of lower end connection refrigerating plant, awkward silence at a meeting lower end temperature is set
- 30 DEG C of degree, 5 DEG C of upper end temperature, moved on to after base substrate freezing completely and ice crystal is removed in freeze drier.After drying, base substrate is shifted
Sintered into vacuum drying oven, being heated to 400 DEG C with 3 DEG C/min speed is incubated 2 hours, removes the binding agent of addition；Further with 5
DEG C/min speed rises to 1200 DEG C of insulation 3h, take out sample after furnace temperature is as cold as room temperature.It is 70% to obtain porosity, directional hole
Interlamellar spacing is~25 μm of POROUS TITANIUM.The aperture of highly directional layered poros is 1.3-3.0cm in sample, the highly directional stratiform hole
The degree of orientation of gap is more than or equal to 90%.
Embodiment 2：
Addition 45g titanium valves, 3g aluminium powders, 4g vanadium powders into ball grinder, 70g deionized waters and 2.1g gelatin (binding agent) mix
After closing liquid ball milling mixing 24h, uniform water base mixed powder slurry is obtained；Water-based slurry injection is placed with and (tilted with inclination angle
Angle be 10 °) adiabatic mould in (square plastic mould), then by mould be put into lower end connection refrigerating plant copper base
On, -20 DEG C of awkward silence at a meeting lower temperature is set, 0 DEG C of upper end temperature, is moved on to after base substrate freezing completely and ice crystal is removed in freeze drier.
After drying, base substrate is transferred in vacuum drying oven and sintered, 350 DEG C of insulation 2h are heated to 5 DEG C/min speed, remove the viscous of addition
Tie agent；1250 DEG C of insulation 2h are further risen to 8 DEG C/min speed, sample is taken out after furnace temperature is as cold as room temperature.Obtain hole
Rate is 60%, and directional hole interlayer aperture is~40 μm porous Ti-6Al-4V (TC4) alloy.The hole of sample orientation layered poros
Footpath is 1.2-2.5cm, and the degree of orientation of the highly directional layered poros is more than or equal to 90%.
Embodiment 3：
The mixed liquor ball milling of 50g titanium valves, 335g deionized waters and 6.7g polyvinyl alcohol (binding agent) is added into ball grinder
After mixing 18h, uniform water base titanium slurry is obtained；Water-based slurry injection is placed with into the heat guard with inclination angle, and (inclination angle is
25 °) in mould (square plastic mould), then mould is put on the copper base of lower end connection refrigerating plant, set under awkward silence at a meeting
- 50 DEG C of temperature is held, -5 DEG C of upper end temperature, is moved on to after base substrate freezing completely and ice crystal is removed in freeze drier.After drying, by base
Body is transferred in argon gas atmosphere and sintered, and being heated to 350 DEG C with 5 DEG C/min speed is incubated 3 hours, removes the binding agent of addition；
1200 DEG C of insulation 2h are further risen to 5 DEG C/min speed, sample is taken out after furnace temperature is as cold as room temperature.Obtaining porosity is
87%, interlayer aperture is~180 μm of POROUS TITANIUM.The aperture of highly directional layered poros is 2.8-7.5cm, the Gao Ding in sample
It is more than or equal to 90% to the degree of orientation of layered poros.
Comparative example
Do not put heat guard
The mixed liquor ball milling mixing of 50gTi powder, 70g deionized waters and 2.1g gelatin (binding agent) is added into ball grinder
After 24h, uniform water base mixed powder slurry is obtained；Water-based slurry is injected in mould, it is cold that mould then is put into lower end connection
Freeze on the copper base of device, -20 DEG C of awkward silence at a meeting lower temperature is set, 0 DEG C of upper end temperature, freeze-drying is moved on to after base substrate freezing completely
Ice crystal is removed in machine.After drying, base substrate is transferred in vacuum drying oven and sintered, 350 DEG C of insulations are heated to 5 DEG C/min speed
2h, remove the binding agent of addition；1250 DEG C of insulation 2h are further risen to 8 DEG C/min speed, taken after furnace temperature is as cold as room temperature
Go out sample.It is 62% to obtain porosity, and directional hole interlayer aperture is~40 μm of porous Ti.Sample laminate hole is along not Tongfang
To without high-orientation.
Claims (8)
- A kind of 1. titanium with high-orientation stratiform orientation interconnected pore；It is characterized in that：The titanium has highly directional layer Shape hole and layer is connected with layer by support frame；The preparation method of the titanium comprises the steps：（1）By metal dust and water mixed liquid by volume 2：98~ 60：40 is well mixed, obtains water-based slurry；The mixing Contain binding agent in liquid, and the quality of binding agent is the 1% ~ 5% of water quality；（2）Water-based slurry injection is placed with the adiabatic mould with inclination angle, it is low in the Double-direction Temperature gradient fields of design Temperature solidification, 30 ~ 50 h of vacuum drying in freeze drying box are put into after slurry completely freezing；Bottom temperature in the orientation temperature field Degree is less than head temperature, and the 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 freeze-drying is removed from the molds, in vacuum or argon gas atmosphere, added with 5 ~ 10 DEG C/min speed Heat is incubated 1 ~ 3 hour to 300 ~ 550 DEG C；Then 1100 ~ 1250 DEG C are risen to 5 ~ 10 DEG C/min speed, insulation 2 ~ 4 h；Furnace cooling obtains the titanium with high-orientation stratiform orientation interconnected pore to room temperature.
- A kind of 2. titanium with high-orientation stratiform orientation interconnected pore according to claim 1；It is characterized in that：Institute The degree of orientation for stating highly directional layered poros is more than or equal to 90%.
- A kind of 3. titanium with high-orientation stratiform orientation interconnected pore according to claim 1；It is characterized in that：Institute State and aperture is also distributed with casing play and/or support frame.
- A kind of 4. titanium with high-orientation stratiform orientation interconnected pore according to claim 1；It is characterized in that：Institute The porosity for stating porous body is 30 ~ 90%.
- A kind of 5. titanium with high-orientation stratiform orientation interconnected pore according to claim 1, it is characterised in that：Institute The granularity for stating metal dust is 0.3 μm~5.0 μm.
- A kind of 6. titanium with high-orientation stratiform orientation interconnected pore according to claim 1, it is characterised in that：The binding agent is selected from least one of gelatin, polyvinyl alcohol, chitosan, polyacrylic acid；The one kind of the material of the adiabatic mould in dimethyl silicone polymer, polyethylene, epoxy resin；The angle change scope of the heat guard is between 5 ~ 25 °.
- 7. a kind of titanium with high-orientation stratiform orientation interconnected pore according to obtained by claim 1-6 any one, it is special Sign is：The titanium is used as bone tissue alternative materials and is applied to the medical domains such as Bone Defect Repari.
- 8. a kind of titanium with high-orientation stratiform orientation interconnected pore according to obtained by claim 1-6 any one, it is special Sign is：The titanium is applied to be separated by filtration field as filtering material；OrAfter the titanium 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 |
| CN110227178A (en) * | 2019-07-30 | 2019-09-13 | 广东工业大学 | A kind of bioceramic scaffold and its application |
| CN110434341A (en) * | 2019-08-30 | 2019-11-12 | 西北有色金属研究院 | A kind of preparation method of full-mesh high porosity nickel-bass alloy material |
| CN110629072A (en) * | 2019-10-10 | 2019-12-31 | 太原理工大学 | Method for preparing porous titanium-aluminum alloy with lamellar structure based on freezing molding process |
| CN110714140A (en) * | 2019-11-20 | 2020-01-21 | 中南大学 | Nickel or nickel alloy porous material with directional holes, preparation method thereof and application thereof in hydrogen evolution electrode |
| CN110732672B (en) * | 2019-12-11 | 2022-05-03 | 中南大学 | Gradient metal-based porous material and preparation method and application thereof |
| CN112553494B (en) * | 2020-11-13 | 2022-03-01 | 南京航空航天大学 | Refrigeration device and method for preparing high-strength and high-toughness layered porous titanium alloy material by using same |
| CN112548100B (en) * | 2020-12-24 | 2022-05-17 | 南京航空航天大学 | Preparation method of bionic oriented ordered laminated composite material |
| 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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| CN103060590B (en) * | 2013-01-08 | 2014-08-06 | 西北工业大学 | Preparation method of gradient porous titanium alloy |
| CN103805797B (en) * | 2014-01-17 | 2016-02-10 | 西北工业大学 | A kind of preparation method of medical porous titanium/porous titanium alloy |
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