CN106178099A - The forming technique of direct write without mould prepares the method for titanium/hydroxylapatite biology support - Google Patents
The forming technique of direct write without mould prepares the method for titanium/hydroxylapatite biology support Download PDFInfo
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- CN106178099A CN106178099A CN201610539398.5A CN201610539398A CN106178099A CN 106178099 A CN106178099 A CN 106178099A CN 201610539398 A CN201610539398 A CN 201610539398A CN 106178099 A CN106178099 A CN 106178099A
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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
- A61L27/12—Phosphorus-containing materials, e.g. apatite
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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
- A61L27/02—Inorganic materials
- A61L27/10—Ceramics or glasses
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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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- 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
- 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 invention provides a kind of method that forming technique of direct write without mould prepares titanium/hydroxylapatite biology support, comprise the following steps: the mixed powder of hydroxyapatite powder and metallic titanium powder is scattered in medium, make titanium/hydroxylapatite ceramic slurry that solid concentration is 50 80wt%；It is pre-designed tomograph by CAD software, and convert thereof into the discernible code language of computer, described titanium/hydroxylapatite ceramic slurry is inserted extrusion syringe, and the path specified along computer under the drive of three-dimensional platform moves, successively extrusion molding simultaneously, forms multilayer order three-dimensional porous network shape structure blank；Described multilayer order three-dimensional porous network shape structure blank is dried, sinters heat treatment step, obtains three dimensional biological support.
Description
Technical field
The invention belongs to medical material tech field, particularly relate to one and prepare titanium/hydroxyl phosphorus without mould direct write forming technique
The method of lime stone biological support.
Background technology
The composition of hydroxyapatite is similar to the inorganic constituents of skeleton with physicochemical property, has good bio-compatible
Property and biological activity, also have induce new bone formation effect, be wide variety of material in lithotroph pottery.Three-dimensional porous hydroxyl
Base apatite structure is largely used to the preparation of biomimic, but, the shortcoming of hydroxylapatite biology support be fragility relatively
Greatly, comprcssive strength low, be only used for non-weight bearing area bone replace.
The forming technique of standard biologic support, needs in forming process to use laser beam or ultraviolet radiation mostly,
Carry out in a heated condition, therefore, its moulding process require higher, condition is relatively harsh and the product that obtains is relatively simple, difficult
To realize the preparation of the product of complicated shape.
Summary of the invention
It is an object of the invention to provide a kind of without mould direct write forming technique prepare titanium/hydroxylapatite biology support and
Method, it is intended to solve to enjoy the moulding process of biological support require higher, condition is relatively harsh, the product that obtains is relatively simple,
Fragility is compared with the problem big, comprcssive strength is low.
The present invention is achieved in that a kind of forming technique of direct write without mould prepares the side of titanium/hydroxylapatite biology support
Method, comprises the following steps:
Being scattered in medium by the mixed powder of hydroxyapatite powder and metallic titanium powder, making solid concentration is 50-
The titanium of 80wt%/hydroxylapatite ceramic slurry；
It is pre-designed tomograph by CAD software, and converts thereof into the discernible code language of computer, by institute
State titanium/hydroxylapatite ceramic slurry and insert extrusion syringe, and the path specified along computer under the drive of three-dimensional platform
Motion, successively extrusion molding simultaneously, form multilayer order three-dimensional porous network shape structure blank；
Described multilayer order three-dimensional porous network shape structure blank is dried, sinters heat treatment step, obtains three-dimensional
Biological support.
And, a kind of biological support prepared by said method, described biological support is by hydroxylapatite powder and metal
The Multilayer Network trellis stereochemical structure of the sintered formation of slurry that titanium valve is mixed into, described hydroxylapatite powder and metallic titanium powder are uniform
It is distributed in the filament of composition grid.
The method that the forming technique of direct write without mould that the present invention provides prepares titanium/hydroxylapatite biology support, on the one hand, by
Near with bone photo in the density of pure titanium, there is good biocompatibility and mechanical performance, and hydroxyapatite has good life
The thing compatibility, therefore, uses the slurry containing hydroxyapatite powder and metallic titanium powder as biological support raw material, it is possible to protecting
On the premise of card biocompatibility, toughness reinforcing hydroxyapatite structure, improve the mechanical performance of biological support, the present invention provides simultaneously
Slurry preparation process simple, the composition of slurry is adjustable；On the other hand, the present invention uses without mould direct write forming technique, molding
Journey need not any laser beam or ultraviolet radiation, without heating, at room temperature can prepare three-dimensional complex shapes
Product.And can be designed by accurate structure without mould direct write forming technique, it is possible to prepare different porosities three-dimensional respectively to
Same sex loose structure, has regulatable comprcssive strength, and also the preparation for three dimensional biological biocompatible scaffold provides more choosing
Select.Additionally, for the feature of different human body skeletal injury, can be designed by structure in advance, for specifically without mould direct writing technology
The individual unique biocompatible scaffold of case custom-made, the good growth and breeding inducing osteocyte.
The biological support that the present invention provides, has preferable biocompatibility and mechanical performance.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of titanium/hydroxylapatite biology support that the embodiment of the present invention provides.
Detailed description of the invention
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearer, below in conjunction with
Embodiment, is further elaborated to the present invention.Should be appreciated that specific embodiment described herein is only in order to explain
The present invention, is not intended to limit the present invention.
Embodiments provide a kind of forming technique of direct write without mould and prepare the side of titanium/hydroxylapatite biology support
Method, comprises the following steps:
S01. being scattered in medium by the mixed powder of hydroxyapatite powder and metallic titanium powder, making solid concentration is
The titanium of 50-80wt%/hydroxylapatite ceramic slurry；
S02. it is pre-designed tomograph by CAD software, and converts thereof into the discernible code language of computer,
Described titanium/hydroxylapatite ceramic slurry is inserted extrusion syringe, and specify along computer under the drive of three-dimensional platform
Move in path, successively extrusion molding simultaneously, forms multilayer order three-dimensional porous network shape structure blank；
S03. described multilayer order three-dimensional porous network shape structure blank is dried, sinters heat treatment step, obtain
Three dimensional biological support.
Concrete, in above-mentioned steps S01, when described hydroxyapatite is separately as biological support, its fragility is big, obtains
Biological rack mechanical poor performance.In view of this, the embodiment of the present invention strengthens described hydroxyapatite by adding other compositions
Toughness, and then improve the mechanical strength of described biological support raw material.The density of pure titanium is near with bone photo, has good biofacies
Capacitive and mechanical performance, but the connection between pure titanium and osseous tissue easily comes off.The embodiment of the present invention is by metallic titanium powder and institute
State hydroxy apatite powder and be mixed with slurry, the effect of toughness reinforcing described hydroxyapatite structure can not only be played, strengthen raw
The mechanical performance of thing support；And can avoid falling off between pure titanium and osseous tissue.Additionally, the embodiment of the present invention can be adjusted
Titanium powder content in control slurry combination structure design in advance, preparation has the periodic network shape biological support of high intensity.
Mixed powder described in the embodiment of the present invention, it is preferred to use following method prepares: by hydroxyapatite powder and
The mixture of Titanium powder, carries out ball-milling treatment for grinding aid by this described mixture with ethanol, and 24-48h is placed on constant temperature
Drying baker, sieves after being dried 24-48h, obtains uniform mixed powder.
In the embodiment of the present invention, in described mixed powder, the content of metallic titanium powder has certain requirement, when described Titanium
When the content of powder is very few, it is not enough to significantly improve the mechanical performance of biological support；When the content of described metallic titanium powder is too much, meeting
Affect the comprcssive strength of sintering temperature and biological support.As the presently preferred embodiments, in described mixed powder, with described mixed powder
Gross weight be 100% meter, the weight percentage of described metallic titanium powder is 30-80%.The more one preferred described Titanium of step
The weight percentage of powder is 50% content, and the intensity of thus obtained biological support is best.
In the embodiment of the present invention, high-performance, stable titanium/hydroxylapatite ceramic slurry are the bases of forming process.This
Titanium described in inventive embodiments/hydroxylapatite ceramic slurry need to meet two important indexs, and first, described slurry to have can
With the viscoelastic response of regulation and control to ensure its smooth extrusion in syringe needle, even and depositing to ensure after on substrate to exist
Also stripe shape and certain span can be maintained the when of below without any support；Second, the shear shinning to be presented of described slurry
Rheological charactristics, it is ensured that the slurry in syringe can be extruded under the effect of shear stress smoothly.Therefore, the embodiment of the present invention
In, on the one hand, the rheological charactristics of described titanium/hydroxylapatite ceramic slurry is shear shinning type；On the other hand, the present invention is real
Executing example with deionized water is that basic solvent can be used for preparing 3 d function pottery to prepare gum size.Concrete, use water base
Gum size, can regulate and control viscoelasticity in the range of multiple orders of magnitude, form the lines of pattern and span.
Concrete, in the embodiment of the present invention, described medium is mixed solvent, and described mixed solvent includes deionized water, divides
Powder and binding agent.Wherein, described dispersant can improve described mixed powder dispersion effect in the medium.Further
Preferably, at least one during described dispersant is ammonium citrate, two citric acid monohydrate trisodiums, methylcellulose.Described bonding
Agent can strengthen the connectivity between described powder body, and then obtain can the slurry of self-sustained.It is further preferred that it is described viscous
Knot agent is at least one in Polyethylene Glycol, polylactic acid, polyvinyl alcohol.It is furthermore preferred that with the gross weight of described medium for 100%
Meter, the content of described dispersant is 0.5-1wt%；The content of described binding agent is 0.5-3wt%.Preferred embodiment the most, institute
State mixed solvent and include deionized water, ammonium citrate, Polyethylene Glycol and polylactic acid, and the content of described ammonium citrate is 0.5-
1wt%；The content of described Polyethylene Glycol and polylactic acid is 0.5-3wt%.This preferred described mixed solvent so that the life obtained
Thing support performance is more uniformly distributed stable.
Described mixed powder is added in described medium by amount by the embodiment of the present invention, it is preferred to use ultrasonic cell disrupte machine shakes
Move to stable homogeneous, obtain homogeneous titanium/hydroxylapatite ceramic slurry system.The embodiment of the present invention is by adding described bonding
Agent and control solid concentration obtain can the slurry of self-sustained, described solid concentration is too low, then cannot realize self-sustained；
Described solid concentration is high, and contraction distortion is little.Additionally, solid concentration can affect the rheological property of slurry.Repeatedly grind through inventor
Studying carefully, the solid concentration of titanium described in the embodiment of the present invention/hydroxylapatite ceramic slurry is 50-80wt%, it is possible to preferably realize
Self-sustained, there is preferable rheological property simultaneously.
In above-mentioned steps S02, the design of rational shape is the basis of whole forming process, and direct write molding is based on discrete-folded
The principle molding added.Discrete additive process is roughly divided into that body is discrete, face is discrete and line is discrete.Body is discrete to be divided 3D solid exactly
Solution becomes continuous print plane, face discrete this be discrete for body go out tangent plane continue to be decomposed into a series of line segment for follow-up molding road
Footpath, final step line is discrete, above-mentioned segment is divided into a series of entity point group, correspond to the minimum unit in molding.This
Bright embodiment uses three-dimensional cylinder network structure, mutually orthogonal between its adjacent two layers, and isotropism can be used for bio-compatible
The preparation of property support.Direct write formation system is made up of three parts: be first computer software, completes the design of figure, and by it
It is converted into code language；Next to that three-dimensional high-precision motion platform, receive the instruction that computer sends, along the road being pre-designed
Move in footpath；It is finally slurry extrusion system, is made up of extrusion syringe, air pressure regulator and gas cylinder, using the teaching of the invention it is possible to provide 1-70psi squeezes
Go out power.
Being pre-designed the figure of three-dimensional yard structure in the embodiment of the present invention, slurry preparation is well inserted capacity later and is
In the syringe of 10ml.Three-dimensional movement platform drives extrusion syringe along set orbiting motion, deposits ground floor on substrate
Structure, then rises to suitable high shape second layer structure along Z axis, is repeated and obtains final three-dimensional yard structure base
Body.Rheological characteristic according to slurry adjusts corresponding extrusion pressure so that it is drop to can solidify rapidly and keep shape on substrate.
The corresponding extrusion pressure of slurry that viscosity is big is relatively big, otherwise, the least.The movement velocity of syringe to match with extrusion pressure, fortune
The when that dynamic speed being little, corresponding extrusion pressure also to be turned down, and pressure the biggest slurry moment extrusion is too much deposited in some position
Put and will cause the asymmetric of total, even subside.The when that syringe needle movement velocity increasing, extrusion pressure to tune up, no
Then pressure is too small, and slurry has little time extrusion, and homogeneous lines interrupt, and cause structure imperfect continuously.Concrete, embodiment is moved
Speed 3-5mm/s, corresponding extrusion pressure is at 40-60psi.
Preferably, formed in the step of multilayer order three-dimensional porous network shape structure blank, use the extrusion of different-diameter
Syringe needle, under the drive of three-dimensional platform, successively write out the cycle with different size parameter along the path pointwise being pre-designed
Property three-dimensional mesh structure.
Having good design and control flexibly without mould direct writing technology described in the embodiment of the present invention, it can basis
Different demands, customize various sizes of biological support, the precision of direct write molding as little as 10 μm.Concrete, described multilayer order three
The design distance between tie rods of dimension porous network shape structure blank is 10-300 μm, lines diameter 10-300 μm.
In above-mentioned steps S03, the multilayer order three-dimensional porous network shape structure blank after molding is placed in low-temperature sintering stove
Carry out preheating, solidify further；Then it is sintered in high temperature sintering furnace.As a preferred embodiment, institute
The method stating preheating is: base substrate is placed in low-temperature sintering stove pre-burning 1-2h at 100-200 DEG C.The most real as another
Executing example, the method for described sintering processes is: the base substrate after low temperature presintering is inserted high temperature furnace, with the intensification of 100-200 DEG C/h
Speed rises to 1100-1300 DEG C of insulation 1-2h sintering processes carried out above from room temperature, cools to room temperature with the furnace and obtains three dimensional biological
Support.As a specific embodiment, rise to from 1200 DEG C of insulation 4h are sintered with the heating rate of 100 DEG C/h from room temperature
Reason.Cooling to room temperature with the furnace and obtain three dimensional biological support, take out sample and characterize, Fig. 1 is outside the three dimensional biological support obtained
Seeing top view, it can be seen that the sample overall structure after sintering is more complete, without significantly deformation, cross section maintains well
Cylindrical.
The method that the forming technique of direct write without mould that the embodiment of the present invention provides prepares titanium/hydroxylapatite biology support, one
Aspect, owing to the density of pure titanium is near with bone photo, has good biocompatibility and mechanical performance, and hydroxyapatite has good
Good biocompatibility, therefore, uses the slurry containing hydroxyapatite powder and metallic titanium powder as biological support raw material, energy
Enough on the premise of ensureing biocompatibility, toughness reinforcing hydroxyapatite structure, improve the mechanical performance of biological support, simultaneously this
The slurry preparation process that bright embodiment provides is simple, and the composition of slurry is adjustable；On the other hand, the embodiment of the present invention uses straight without mould
Write forming technology, need not any laser beam or ultraviolet radiation in forming process, without heating, at room temperature can make
For going out three-dimensional complex shapes product.And can be designed by accurate structure without mould direct write forming technique, it is possible to prepare difference
The Three-Dimensional Isotropic loose structure of porosity, has regulatable comprcssive strength, is also the system of three dimensional biological biocompatible scaffold
For providing more choices.Additionally, for the feature of different human body skeletal injury, can pass through in advance without mould direct writing technology
Structure designs, for the concrete individual unique biocompatible scaffold of case custom-made, the good growth inducing osteocyte
Breeding.
In real life, the most all can occur much must treating by transplanting skeleton or installation neologism
The accident of damage, such as vehicle accident, the industry reason such as accident, traumatic injury, cancer even face-lifting excise skeleton, without mould direct write molding
Technology can be that concrete individual case customizes unique biocompatible scaffold, and then effectively induces determining of osteocyte
To growth, the life and health for the mankind is made huge contribution.
And, the embodiment of the present invention additionally provides a kind of biological support prepared by said method, and described biological support is
The sintered Multilayer Network trellis stereochemical structure formed of slurry being mixed into by hydroxylapatite powder and metallic titanium powder, described hydroxyl phosphorus
Limestone flour and metallic titanium powder are uniformly distributed in the filament of composition grid.
The biological support that the embodiment of the present invention provides, has preferable biocompatibility and mechanical performance.
Two kinds of compositions are uniformly distributed in the filament of composition grid, connect good, nothing between intersection's levels of grid
Slurry is piled up and is subsided.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (10)
1. the method preparing titanium/hydroxylapatite biology support without mould direct write forming technique, comprises the following steps:
Being scattered in medium by the mixed powder of hydroxyapatite powder and metallic titanium powder, making solid concentration is 50-80wt%
Titanium/hydroxylapatite ceramic slurry；
It is pre-designed tomograph by CAD software, and converts thereof into the discernible code language of computer, by described
Extrusion syringe inserted by titanium/hydroxylapatite ceramic slurry, and along the path fortune that computer is specified under the drive of three-dimensional platform
Dynamic, successively extrusion molding simultaneously, form multilayer order three-dimensional porous network shape structure blank；
Described multilayer order three-dimensional porous network shape structure blank is dried, sinters heat treatment step, obtains three dimensional biological
Support.
2. the method preparing titanium/hydroxylapatite biology support without mould direct write forming technique as claimed in claim 1, its feature
Being, in described mixed powder, be in terms of 100% by the gross weight of described mixed powder, the weight percent of described metallic titanium powder contains
Amount is 30-80%.
3. the method preparing titanium/hydroxylapatite biology support without mould direct write forming technique as claimed in claim 1, its feature
Being, described medium is mixed solvent, and described mixed solvent includes deionized water, dispersant and binding agent.
4. the method preparing titanium/hydroxylapatite biology support without mould direct write forming technique as claimed in claim 3, its feature
Being, described dispersant is at least one in ammonium citrate, two citric acid monohydrate trisodiums, methylcellulose, described binding agent
For at least one in Polyethylene Glycol, polylactic acid, polyvinyl alcohol, and it is in terms of 100% by the gross weight of described medium, described dispersion
The content of agent is 0.5-1wt%；The content of described binding agent is 0.5-3wt%.
5. the method that the forming technique of direct write without mould as described in claim 1-4 is arbitrary prepares titanium/hydroxylapatite biology support,
It is characterized in that, the rheological charactristics of described titanium/hydroxylapatite ceramic slurry is shear shinning type.
6. the method that the forming technique of direct write without mould as described in claim 1-4 is arbitrary prepares titanium/hydroxylapatite biology support,
It is characterized in that, formed multilayer order three-dimensional porous network shape structure blank step in, use different-diameter extrusion syringe needle,
Successively write out the periodicity three with different size parameter along the path pointwise being pre-designed under the drive of three-dimensional platform
Dimension fenestral fabric.
7. the method that the forming technique of direct write without mould as described in claim 1-4 is arbitrary prepares titanium/hydroxylapatite biology support,
It is characterized in that, the design distance between tie rods of described multilayer order three-dimensional porous network shape structure blank is 10-300 μm, lines diameter
10-300μm。
8. the method that the forming technique of direct write without mould as described in claim 1-4 is arbitrary prepares titanium/hydroxylapatite biology support,
It is characterized in that, before described heat treatment is additionally included in sintering, base substrate is placed in low-temperature sintering stove pre-burning 1-at 100-200 DEG C
2h, solidifies further.
9. the method preparing titanium/hydroxylapatite biology support without mould direct write forming technique as claimed in claim 8, its feature
Being, the base substrate after described heat treatment includes low temperature presintering inserts high temperature furnace, with the heating rate of 100-200 DEG C/h from room
Temperature rise, to 1100-1300 DEG C of insulation 1-2h sintering processes carried out above, cools to room temperature with the furnace and obtains three dimensional biological support.
10. the biological support prepared according to method described in claim 1-9 any one, it is characterised in that described biology
Support is the sintered Multilayer Network trellis stereochemical structure formed of the slurry being mixed into by hydroxylapatite powder and metallic titanium powder, described
Hydroxylapatite powder and metallic titanium powder are uniformly distributed in the filament of composition grid.
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| CN115957374A (en) * | 2022-12-16 | 2023-04-14 | 吉林大学 | Metal artificial bone implant with core-shell structure and preparation method thereof |
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