CN103462729A - Preparation method of bionic artificial bone with multistage [micrometer/nanometer] pore structure - Google Patents
Preparation method of bionic artificial bone with multistage [micrometer/nanometer] pore structure Download PDFInfo
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Abstract
The invention relates to a preparation method of a bionic artificial bone with a multistage [micrometer/nanometer] pore structure. The method is characterized by the following steps of: realizing 150-800 mum gradient through pores by selective laser sintering (the diameter of the light spot is micrometer scale); mixing and performing oxygenolysis on a small amount of high polymer microballoons in the sintering process to form 10-100 mum random spherical pores; finally obtaining the bionic artificial bone which has an three-dimensional hierarchical pore structure similar to that of a natural bone by a method of obtaining irregular pores in tens of nanometer surfaces by a corrosion process. In the invention, according to the requirement of an implanting position, the distribution, connectivity and the like of the gradient through pore can be accurately controlled by adjusting sintering process parameters; the shape, size and the like of the spherical pores can be controlled by precisely controlling the furnace temperature curve and high polymer particle properties; the size, quantity and the like of the nanometer pores can be controlled by controlling the corrosion liquid concentration and corrosion time. The preparation method disclosed by the invention has an important significance in creating a microenvironment beneficial to cell adhesion, proliferation and function exertion, improving forming of new bones, and increasing healing of bones.
Description
Technical field
The invention belongs to the bionical manufacture field of bone tissue engineer, particularly when preparing the biomimetic artificial bone of hierarchical porous structure, provide a kind of and utilize selective laser sintering to realize 150-800 μ m gradient through hole, a small amount of high polymer micro balloons oxidation Decomposition in sintering process of utilize mixing forms the random spherical pore of 10-100 μ m, utilize etching process to obtain the method in tens nanometer surface imperfection hole, finally obtains having the biomimetic artificial bone with the similar three-dimensional multistage pore structure of autologous bone.
Technical background
The disappearance of tissue or dysfunction are the significant problems that threatens human health, are also the ill and dead main reasons of the mankind.Particularly in recent years along with aged tendency of population, and the development of the causes such as industry, traffic, physical culture, it is day by day urgent that the reparation that people are damaged to osseous tissue and replacing requires.For a long time, the bone graft of clinical middle use mainly contains autologous bone and allograph bone, but autologous bone transplanting limitedly can't meet requirement that large section bone transplant and the damaged case of bone on a large scale owing to drawing materials, and allogenic bone transplantation slowly affects patient's functional rehabilitation owing to being substituted process, so people thirst for obtaining the auxiliary new osteanagenesis of a kind of energy and source is sufficient, the short biomimetic artificial bone of healing time.
Desirable biomimetic artificial bone not only will be for defect provides support structure, the more important thing is and will create a kind of microenvironment that is conducive to cell adhesion, proliferation and function performance, induces osteocyte to generate, and degraded and absorbed gradually, finally forms new bone.This requires the biomimetic artificial bone support to possess good biocompatibility and biological activity, and has the microcosmic loose structure of applicable growth and proliferation of cell, and with the identical profile of defect and enough mechanical strengths etc.Bioactive ceramics mainly comprises hydroxyapatite (HAP), calcium phosphate (TCP) and bio-vitric (BG) etc., owing to thering is good biocompatibility, degradability and bone conductibility, show good affinity with cell, be considered to current most potential bone alternate material.
How realizing that the three-dimensional porous structure consistent with natural bone is suitable for the microenvironment of cellular activity, procreation with creation, is the key that can artificial bone scaffold bring into play optimum skeletonization usefulness.Natural bone is a kind of material with three-dimensional multistage pore structure, aperture is from tens nanometer to hundreds of microns, can meet the growth requirement of different tissues, wherein the aperture of 150-800 μ m is conducive to osseous tissue, growing into of blood vessel, the aperture of 10-100 μ m allows growing into of blood capillary, promote the exchange of nutrient substance and the discharge of metabolite, the aperture of nanoscale can provide larger specific surface area and more active target spot, the forming core and the protein that are conducive to apatite, osteoblastic absorption, adhesion and the migration propagation of cell are had to important regulating action simultaneously.The structure in this three-dimensional multistage hole has proposed great challenge to the bionical manufacture of artificial bone scaffold.
The traditional method for preparing at present loose structure mainly contains chemical blowing process, adds pore creating material method, half sintering reaming method, organic backbone duplicating method, sintering microsphere method etc.Chemical blowing process is that material and the ceramic powders mixed-forming that chemical reaction produces gas can at high temperature occur, and processes at a certain temperature foaming and produces porous ceramics; The pore creating material method is by add pore creating material in pottery, makes its at high temperature after-flame or volatilization and stay hole in pottery; Half sintering reaming method is that half sintered body is soaked after reaming to double sintering again; The organic backbone duplicating method is to adopt to have the hole Corallium Japonicum Kishinouye of similar cancellous bone structure as artificial bone; Sintering microsphere method is that degradable polymer microspheres is added in mould, more than being heated to vitrification point, through insulation, cooling, the demoulding, makes porous support; Be separated/Emulsion freeze-drying is that polymer solution, emulsion etc. is separated through freezing, thereby then utilize freeze drying process to remove solvent, obtains porous support.Above-mentioned these methods lack the control to pore structure (as pore size, space trend and connectedness etc.), the more important thing is that pore structure is single, can't meet the growth requirement of different tissues, and pore structure is compared and still had larger difference with natural bone.
In sum, seek the bionic preparation that an effective technological approaches is realized artificial bone scaffold three-dimensional multistage hole, to meet the growth requirement of different cells in the bone repair process, have great importance for new osteanagenesis healing acceleration time.
Summary of the invention
Deficiency and the single problem of structure pore structure controlled for existing method, the present invention proposes a kind of utilize selective laser (spot diameter is micro-meter scale) sintering realize 150-800 μ m gradient through hole, a small amount of high polymer micro balloons utilize mixed and in sintering process oxidation Decomposition form the random spherical pore of 10-100 μ m, utilize etching process to obtain the method in tens nanometer surface imperfection hole, finally obtain having the biomimetic artificial bone with the similar three-dimensional multistage pore structure of natural bone.
The preparation method that has the biomimetic artificial bone of hierarchical porous structure in the present invention mainly comprises the following steps:
(1) raw material preparation: add a certain amount of high polymer (polylactic acid (PLA), poly-acetic acid (PGA) and copolymer (PLGA) thereof etc.) microsphere in the nano-bioactive ceramic powders, obtain mixed uniformly powder by mechanical mixing, wherein the mass fraction of high polymer is 10-40%.
(2) green compact molding: lay uniformly one deck mixed-powder on sintering platform, powder layer thickness is 0.15-0.2mm, control laser beam according to support two-dimensional section information and selectively scan sintered powder, by the technology that is layering, obtain three-dimensional bionic artificial bone scaffold green compact.
(3) clear powder is processed: sintering platform certain height that descends, after utilizing the equipment such as hairbrush, compressor, air gun or vacuum cleaner to remove unsintered powder, obtains the gradient through hole of 150-800 μ m.
(4) high temperature sintering: the green compact after clear powder are seated in temperature controlling stove to sintering again, and control by precision the random spherical pore that removal that the furnace temperature curve carries out high polymer forms 10-100 μ m simultaneously.
(5) acid and alkali corrosion: the biomimetic artificial bone support is immersed in certain density acidity or alkaline solution and carries out chemical attack, after certain hour, support is taken out, utilize deionized water rinsing and dry, obtain the surface imperfection hole of nanoscale.
Compared with prior art, advantage of the present invention is:
(1) utilize micron order laser facula (50 μ m) selectively sintered powder can obtain 150-800 μ m and run through fully gradient pore structured.According to the implant site requirement, by adjusting the technological parameters such as laser power, sweep span, spot size, sintering path, can accurately control the distribution, connectedness, porosity of gradient through hole etc.
(2) again in sintering process high polymer micro balloons gradually oxidation Decomposition, discharge until disappear fully, the final random spherical pore that forms 10-100 μ m in nano ceramics.According to the implant site requirement, by shape, size and the content of controlling the high polymer granule, can control the size of formed spherical pore and quantity etc.
(3) utilize etching process to carry out acid-alkali treatment to the nano-bioactive ceramics bracket, obtain the netted hole of nanoscale by changing the rack surface pattern.According to the implant site requirement, by controlling corrosive liquid concentration and etching time, can control the size of nano-pore and quantity etc.
(4) a kind of controllable method for preparing of biomimetic artificial bone three-dimensional multistage pore structure has been proposed, comprise hundreds of microns gradient through holes, the random spherical pore of tens of micron and tens nanometer surface imperfection hole, and can pass through the adjusting process gain of parameter three-dimensional porous structure consistent with natural bone.
The accompanying drawing explanation
Fig. 1 is independently developed selective laser sintering system.
Fig. 2 is hundreds of microns gradient through holes that utilize the micron order laser facula to prepare.
Fig. 3 utilizes the high polymer micro balloons random spherical pore of tens of microns that oxidation Decomposition obtains in sintering process.
Fig. 4 is the tens nanometer surface imperfection hole that utilizes etching process to obtain.
The specific embodiment
Below by an example, the specific embodiment of the present invention is set forth:
Adopting nanometer hydroxyapatite powder and Poly-L-lactic acid PLLA is raw material, and wherein HAP is the minute hand shape, is about 150nm, wide about 20nm, mean diameter 40nm; The PLLA mean diameter is 10-100 μ m, and relative viscosity is 0.51-1.0dl/g.Method by mechanical mixture obtains mixed uniformly PLLA/HAP powder stock, and wherein the PLLA mass fraction is 10%.Based on independently developed selective laser sintering system, the sinter molding of carrying out the PLLA/HAP powder under the process conditions of laser spot diameter 50 μ m, paving powder thickness 0.2 μ m obtains the support green compact, green compact are seated in temperature controlling stove and carry out sintering more again, and control the furnace temperature curve by precision and remove the PLLA in green compact.Again support is put into to the corrosion of Fluohydric acid. (HF) solution that concentration is 10% and taken out after 10 minutes, with deionized water rinsing 5 minutes and put into 40 ℃ of baking ovens and dry.
Utilize scanning electron microscope (SEM) to test and analyze the pore structure of support.In Fig. 2, the hole of hundreds of microns run through fully and porosity higher; Fig. 3 shows in support to have the spherical pore of tens of microns, and distribution uniform; Can find out in Fig. 4 that there are a large amount of irregular holes in rack surface after corrosion, size is that tens nanometers do not wait to tens nanometer.Result of study has confirmed that the present invention can utilize selective laser (spot diameter is micro-meter scale) sintering to realize the preparation of 150-800 μ m gradient through hole, utilize a small amount of high polymer micro balloons oxidation Decomposition in sintering process of mixing to form the random spherical pore of 10-100 μ m, utilize etching process to form tens nanometer surface imperfection pore structure, the biomimetic artificial bone of final acquisition and the similar loose structure of natural bone, this is for promoting new bone formation, quickening knitting to have great importance.
Claims (5)
1. a small amount of high polymer micro balloons oxidation Decomposition in sintering process of utilizing selective laser (spot diameter is micro-meter scale) sintering to realize that 150-800 μ m gradient through hole, utilization mix forms the random spherical pore of 10-100 μ m, utilizes etching process to obtain the method in tens nanometer surface imperfection hole, finally obtain having the biomimetic artificial bone with the similar three-dimensional multistage pore structure of natural bone, key step comprises:
(1) raw material preparation: add a certain amount of high polymer (polylactic acid (PLA), poly-acetic acid (PGA) and copolymer (PLGA) thereof etc.) microsphere in the nano-bioactive ceramic powders, obtain mixed uniformly powder by mechanical mixing, wherein the mass fraction of high polymer is 10-40%;
(2) green compact molding: lay uniformly one deck mixed-powder on sintering platform, powder layer thickness is 0.15-0.2mm, control laser beam according to support two-dimensional section information and selectively scan sintered powder, by the technology that is layering, obtain three-dimensional bionic artificial bone scaffold green compact;
(3) clear powder is processed: sintering platform certain height that descends, after utilizing the equipment such as hairbrush, compressor, air gun or vacuum cleaner to remove unsintered powder, obtains the gradient through hole of 150-800 μ m;
(4) high temperature sintering: the green compact after clear powder are seated in temperature controlling stove to sintering again, and control by precision the random spherical pore that removal that the furnace temperature curve carries out high polymer forms 10-100 μ m simultaneously;
(5) acid and alkali corrosion: the biomimetic artificial bone support is immersed in certain density acidity or alkaline solution and carries out chemical attack, after certain hour, support is taken out, utilize deionized water rinsing and dry, obtain the surface imperfection hole of nanoscale.
2. according to the method for preparing the three-dimensional multistage pore structure described in claim 1, it is characterized in that: utilize micro-meter scale laser facula (50 μ m) selectively sintered powder can obtain 150-800 μ m and run through fully gradient pore structured, according to the implant site requirement, by adjusting the technological parameters such as laser power, sweep span, spot size, sintering path, can accurately control the distribution, connectedness, porosity of gradient through hole etc.
3. according to the method for preparing the three-dimensional multistage pore structure described in claim 1, it is characterized in that: in sintering process high polymer micro balloons gradually oxidation Decomposition, discharge until disappear fully, the final random spherical pore that forms 10-100 μ m in nano ceramics, according to the implant site requirement, by shape, size and the content of controlling the high polymer granule, can control the shape of formed spherical pore and size etc.
4. according to the method for preparing the three-dimensional multistage pore structure described in claim 1, it is characterized in that: utilize etching process to carry out acid-alkali treatment to the nano-bioactive ceramics bracket, obtain the netted hole of nanoscale by changing the rack surface pattern, according to the implant site requirement, can control the size and number of nano-pore etc. by control corrosive liquid concentration and etching time.
5. according to the method for preparing the three-dimensional multistage pore structure described in claim 1, it is characterized in that: the controllable method for preparing that has proposed a kind of biomimetic artificial bone three-dimensional multistage pore structure, comprise hundreds of microns gradient through holes, the random spherical pore of tens of micron and nanoscale surface imperfection hole, and can pass through the adjusting process gain of parameter three-dimensional porous structure consistent with natural bone.
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| CN106620882A (en) * | 2016-11-18 | 2017-05-10 | 北京积水潭医院 | Artificial bone structure having density gradient |
| CN106624369A (en) * | 2016-10-14 | 2017-05-10 | 清华大学 | Method for quickly preparing oxide multi-stage nanostructure |
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| CN106880424A (en) * | 2015-12-16 | 2017-06-23 | 重庆润泽医药有限公司 | A kind of artificial shoulder joint prosthesis |
| CN108144113A (en) * | 2018-02-12 | 2018-06-12 | 华南理工大学 | A kind of porous bone repair material of bioactivity glass and preparation method thereof |
| CN109806032A (en) * | 2019-03-22 | 2019-05-28 | 河北雄安大洲智造科技有限公司 | A kind of porous tantalum stick and preparation method thereof |
| CN109809811A (en) * | 2019-03-13 | 2019-05-28 | 华南理工大学 | A kind of bioactive ceramics bracket of Nano/micron hierarchical porous structure and preparation method thereof |
| CN110614369A (en) * | 2018-06-20 | 2019-12-27 | 韩国生产技术研究院 | One-step method for producing a laminated porous member |
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| CN112296355A (en) * | 2020-09-26 | 2021-02-02 | 四川大学 | Method for manufacturing titanium alloy bone tissue engineering implant with micron-sized topological porous structure by SLM (Selective laser melting) |
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| CN110614369A (en) * | 2018-06-20 | 2019-12-27 | 韩国生产技术研究院 | One-step method for producing a laminated porous member |
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| CN109809811B (en) * | 2019-03-13 | 2021-09-21 | 华南理工大学 | Bioactive ceramic support with nano/micron hierarchical pore structure and preparation method thereof |
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| CN112296355A (en) * | 2020-09-26 | 2021-02-02 | 四川大学 | Method for manufacturing titanium alloy bone tissue engineering implant with micron-sized topological porous structure by SLM (Selective laser melting) |
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| CN112972764A (en) * | 2021-03-19 | 2021-06-18 | 吉林大学 | Polyether-ether-ketone bone repair material with multi-scale holes and preparation method thereof |
| CN112972764B (en) * | 2021-03-19 | 2022-04-26 | 吉林大学 | Polyether-ether-ketone bone repair material with multi-scale holes and preparation method thereof |
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