CN103740963B - Method for preparing porous tantalum medical implant material by selective laser sintering formation - Google Patents
Method for preparing porous tantalum medical implant material by selective laser sintering formation Download PDFInfo
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Abstract
The invention relates to a preparation method of a porous tantalum medical implant material. The preparation method comprises the following steps: by adopting pure tantalum powder with the particle size of not more than 10mu m as a raw material, directly performing selective laser sintering formation to form a human bone metal biomimetic material, wherein the thickness of powder spread in each layer during selective laser sintering is 60-80mu m; further sintering and cooling the formed human bone metal biomimetic material to obtain the porous tantalum medical implant material. The porous tantalum medical implant material with complete three-dimensional communication is obtained by sintering and cooling treatment of a formed blank prepared by selective laser sintering, and has a consistent microstructure with a bone tissue of a human body, so that the porous metal implant material has good biocompatibility and biological safety. The method provided by the invention further has the advantages of simple process equipment, low operation cost, no pollution in the whole preparation process, no side effect on a human body, capacity of ensuring the biological safety of the implant material and high forming speed, and is very conductive to industrial production and application.
Description
The present patent application is application number 201210022123.6, the applying date on 01 31st, 2012, the divisional application of denomination of invention " a kind of adopt the shaping method preparing porous tantalum medical embedded material of selective laser sintering ".
Technical field
The present invention relates to the preparation field of porous medical metal implanted material, particularly a kind of method adopting selective laser sintering technology to prepare porous medical metal implanted material.
Background technology
Porous medical metal implanted material has the important and special purposes such as treatment osseous tissue wound and bone formation necrosis, and existing common this kind of material has metal stainless steel, porous metal titanium etc.As the porous embedded material that osseous tissue wound and bone formation necrosis therapeutic use, its porosity should reach 30 ~ 80%, and hole is preferably all communicated with and is uniformly distributed, or aperture sections is communicated with and is uniformly distributed as required, make it both consistent with the bone growth of human body, alleviate again the weight of material itself, implant with applicable human body and use.
And refractory metals tantalum, because it has outstanding biocompatibility and mechanical property, its porous material is expected to the conventional medical metallic biomaterial such as aforementioned as an alternative, becomes the biomaterial mainly as bone necrosis's treatment.Due to metal tantalum to human body harmless, nontoxic, have no side effect, and along with the develop rapidly of domestic and international medical science, to tantalum going deep into further as body implanting material cognition, the demand of people to human body porous metal tantalum material becomes more and more urgent, also more and more higher to its requirement.Wherein as porous medical metal tantalum, if the very high physical and mechanical properties being uniformly distributed open pore and adapting with human body can be had, then it is the heavy connection constituent material ensureing freshman bone tissue's normal growth.
The preparation method of current porous tantalum biomaterial mainly contains powder loose sintering method, foam impregnation sintering process, slurry foaming etc., and these methods all need to apply mould.And the maximum feature of biomaterial is complex-shaped, high to small detail, therefore, very high requirement is proposed to forming technique, but traditional forming technique cannot meet the demands owing to being subject to the restriction of mould.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of simple and efficient, porous tantalum medical embedded material that cost is low, obtained porous tantalum medical embedded material good biocompatibility.
The object of the invention is achieved by the following scheme:
A kind of preparation method of porous tantalum medical embedded material, it is characterized in that: adopt particle diameter≤10 μm (preferably adopting 5 ~ 10 μm of pure tantalum powder) pure tantalum powder to be raw material, directly carry out selective laser sintering shaping people's bone metal biomimetic material, during selective laser sintering, the paving powder thickness of every layer is at 60 ~ 80 μm; Again sintering is comprised to shaping people's bone metal biomimetic material, cooling obtains porous tantalum medical embedded material.
The forming blank adopting above-mentioned selective laser sintering to obtain obtains the porous tantalum medical embedded material, consistent with body bone tissue microtexture of the complete three-dimensional communication of hole through sintering, cooling process, makes this porous metal embedded material biocompatibility, biological safety good.According to the needs of corresponding implantation, the present invention also by regulate selective laser sintering shaping and sintering processing parameter control final porous tantalum porosity, make the osseous tissue that its mechanical property is corresponding to human body consistent simultaneously, avoid porous tantalum not mate with body mechanics's performance and the stress concentration caused thus affect the long-term effect of implant, meet different requirements with this; Alternative human bearing position osseous tissue can be prepared as porous tantalum embedded materials such as femur, face stocks as regulated and controled corresponding process parameters, also can prepare the porous tantalum embedded material of alternative human body non-bearing osseous tissue.The laser sintered device adopted in selective laser sintering method of the present invention is known, selective laser sintering technology (SLS) is a kind of technology based on laser sintered rapid shaping, adopt laser layering sintering solid powder selectively, and the cured layer of sinter molding is layering generate the sample of desired shape, its whole technological process comprises foundation and data processing, paving powder, the thermal sintering etc. of three-dimensional model, at present, the material that successfully can carry out SLS forming process has paraffin, polymer, metal, ceramic powder and their composite powder material.Can adjust the shape of molded samples as required, the use of selective laser sintering device is input in molding device software kit by the three-dimensional model file designed to carry out selective laser sintering, and this is this area routine techniques.The inventive method also has that processing unit is simple, running cost is low, whole preparation process is pollution-free, without any side effects to human body, be beneficial to the biological safety ensureing embedded material, shaping speed is beneficial to suitability for industrialized production application soon, very much simultaneously.
Further; in order to the obtained porous tantalum medical embedded material being suitable for alternative human bearing's osseous tissue; the preferred processing parameter of selective laser sintering moulding process of the present invention is: laser power is at 50 ~ 65W; sweep velocity is 15 ~ 25mm/s; sweep span is 0.05 ~ 0.15mm; every layer spreads bisque thick is 60 ~ 80 μm, and whole moulding process is carried out in argon atmosphere, and purity of argon is greater than 99.999%.
More particularly, the preparation method of porous tantalum medical embedded material of the present invention is specific as follows:
1, selective laser sintering is shaping: be that 5 ~ 10 μm of pure tantalum powder are transported on shaped platform by particle diameter, roll extrusion laying, then the UG three-dimensional model file of the porous tantalum embedded material designed is input to molding device software kit, and carries out selective laser sintering; The processing parameter of selective laser sintering is: laser power is at 50 ~ 65W, sweep velocity is 15 ~ 25mm/s, and sweep span is 0.05 ~ 0.15mm, and every layer spreads bisque thick is 60 ~ 80 μm, whole moulding process is carried out in argon atmosphere, and purity of argon is greater than 99.999%;
2, the vacuum sintering of above-mentioned gained shaping blank, cooling: first stage is the high-temperature vacuum sintering stage, rises to 1200 ~ 1250 DEG C with the speed of 10 ~ 15 DEG C/min, insulation 30 ~ 60min, vacuum tightness is 10
-4pa ~ 10
-3pa; Rise to 1500 DEG C with the speed of 10 ~ 20 DEG C/min, insulation 30 ~ 60min, vacuum tightness is 10
-4pa ~ 10
-3pa, rises to 2000 ~ 2200 DEG C with the speed of 6 ~ 20 DEG C/min, and insulation 120 ~ 240min, vacuum tightness is 10
-4pa ~ 10
-3pa; Second stage is the Slow cooling stage, and vacuum tightness is 10
-4pa ~ 10
-3pa; 1500 ~ 1600 DEG C are cooled to, insulation 30 ~ 60min with the speed of 10 ~ 20 DEG C/min; 1200 ~ 1250 DEG C are cooled to, insulation 60 ~ 90min with the speed of 12 ~ 20 DEG C/min; 800 DEG C are cooled to, then furnace cooling with the speed of 10 ~ 20 DEG C/min.
In order to sinter evenly, thorough, make the porous tantalum embedded material obdurability that obtains better, be suitable as alternative human bearing position osseous tissue as porous tantalum embedded materials such as femur, face stocks, the above-mentioned sintering process to shaping blank preferably carries out as follows: be 10 in vacuum tightness
-4pa ~ 10
-3pa, be warming up to 1500 ~ 1800 DEG C with 10 ~ 20 DEG C/min, be incubated 120 ~ 240min, be chilled to 200 ~ 300 DEG C with stove, be warming up to 1500 ~ 1800 DEG C, insulation 180 ~ 240min with 10 ~ 20 DEG C/min again, be warming up to 2000 ~ 2200 DEG C, insulation 120 ~ 360min with 5 ~ 10 DEG C/min.
In order to eliminate more fully porous tantalum embedded material internal stress, make it organize evenly, improve toughness further, above-mentioned sintering, cooling after also carry out anneal, described annealing process step is vacuum tightness is 10
-4pa ~ 10
-3pa, is warming up to 800 ~ 900 DEG C, insulation 240 ~ 480min with 10 ~ 20 DEG C/min, then is chilled to 400 DEG C, insulation 120 ~ 300min with 2 ~ 5 DEG C/min, then cools to room temperature with the furnace.
The selective laser sintering device that selective laser sintering moulding process of the present invention adopts is made up of powder cylinder and moulding cylinder, during work, powder cylinder piston (powder feeding piston) rises, by powder-laying roller by powder uniform spreading last layer on moulding cylinder piston (working piston), computer controls the two-dimensional scan track of laser beam according to the hierarchical model of prototype, sinters the pure tantalum powder of conveying selectively to form an aspect of part.After powder completes one deck, working piston declines a thickness, paving powder system spreads new tantalum powder, controls laser beam and scans the new layer of sintering again, so move in circles, be layering, until three-dimensional samples is shaping, finally, by unsintered Powder Recovery in powder cylinder, and take out profiled member and obtain shaping blank, whole selective laser sintering is in a vacuum environment.
Most preferably, a kind of method preparing porous tantalum medical embedded material, carry out according to the following steps:
1, selective laser sintering is shaping: be that 5 ~ 10 μm of pure tantalum powder are transported on shaped platform by particle diameter, roll extrusion laying, then the UG three-dimensional model file of the porous tantalum embedded material designed is input to molding device software kit, and carries out selective laser sintering; The processing parameter of selective laser sintering is: laser power is at 55 ~ 60W, sweep velocity is 15 ~ 25mm/s, and sweep span is 0.05 ~ 0.15mm, and every layer spreads bisque thick is 70 ~ 75 μm, whole moulding process is carried out in argon atmosphere, and purity of argon is greater than 99.999%;
2, the vacuum sintering of above-mentioned gained shaping blank, cooling, annealing: first stage is the high-temperature vacuum sintering stage, is 10 in vacuum tightness
-4pa ~ 10
-3pa, be warming up to 1500 ~ 1800 DEG C with 10 ~ 20 DEG C/min, be incubated 120 ~ 240min, be chilled to 200 ~ 300 DEG C with stove, be warming up to 1500 ~ 1800 DEG C, insulation 180 ~ 240min with 10 ~ 20 DEG C/min again, be warming up to 2000 ~ 2200 DEG C, insulation 120 ~ 360min with 5 ~ 10 DEG C/min; Second stage is the Slow cooling stage, and vacuum tightness is 10
-4pa ~ 10
-3pa; 1500 ~ 1600 DEG C are cooled to, insulation 30 ~ 60min with the speed of 10 ~ 20 DEG C/min; 1200 ~ 1250 DEG C are cooled to, insulation 60 ~ 90min with the speed of 12 ~ 20 DEG C/min; 800 DEG C are cooled to, then furnace cooling with the speed of 10 ~ 20 DEG C/min; Three phases is annealing, and vacuum tightness is 10
-4pa ~ 10
-3pa, is warming up to 800 ~ 900 DEG C, insulation 240 ~ 480min with 10 ~ 20 DEG C/min, then is chilled to 400 DEG C, insulation 120 ~ 300min with 2 ~ 5 DEG C/min, then cools to room temperature with the furnace.
The present invention has following beneficial effect:
The porous tantalum medical embedded material that selective laser sintering moulding process of the present invention obtains achieves the complete three-dimensional communication of hole, it is consistent with body bone tissue microtexture, biocompatibility, the biological safety of material are excellent, and present method also achieves the shape adjusting blank sample as required flexibly simultaneously.In conjunction with techniques such as preferred sintering aftertreatments, the porous tantalum medical embedded material density that the present invention obtains can reach 5.00 ~ 7.00g/cm
3, the dispersity of hole is high, porosity can reach 60 ~ 80%, the complete three-dimensional communication of hole and be evenly distributed, good biocompatibility, aperture can at 200 μm ~ 400 μm; Young's modulus can reach 5.0 ~ 6.5Gpa, flexural strength can reach 125 ~ 145Mpa, ultimate compression strength can reach 80 ~ 90Mpa, is suitable as very much the embedded material of alternative human bearing's osseous tissue.Moreover preparation method's technique of the present invention simply, is easily controlled; Whole preparation process is harmless, pollution-free, toxicological harmless dust, without any side effects to human body.
Accompanying drawing explanation
Fig. 1 is the vertical microscope analysis chart that preparation method of the present invention obtains the microtexture of porous tantalum; Can be observed from accompanying drawing: the complete three-dimensional communication of porous tantalum hole that the present invention obtains, and be evenly distributed.
Embodiment
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is that following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, person skilled in art can make some nonessential improvement and adjustment according to the invention described above content to the present invention.
Embodiment 1
A kind of preparation method of porous tantalum medical embedded material, be that the pure tantalum powder of 5 μm is transported on the platform of 3 D-printing by particle diameter, roll extrusion laying, designing the sample size that will prepare is φ 10 × 100mm, and by its UG file molding equipment, it is shaping to carry out selective laser sintering.Computer controls the two-dimensional scan track of laser beam according to the hierarchical model of prototype, sinter the pure tantalum powder of conveying selectively to form an aspect of part, after powder completes one deck, working piston declines 50 μm, paving powder system spreads new tantalum powder, every layer to spread bisque thick be 80 μm, controls laser beam and scans the new layer of sintering again, so move in circles, be layering, until three-dimensional samples is shaping.Then take out molded samples, put into vacuum oven and carry out high-temperature vacuum sintering, rise to 1200 DEG C with the speed of 10 ~ 15 DEG C/min from room temperature, insulation 1.0h, vacuum tightness is 1 × 10
-4pa; Rise to 1500 DEG C with the speed of 10 DEG C/min, insulation 1.0h, vacuum tightness is 1 × 10
-4pa ~ 1 × 10
-3pa; Rise to 2100 DEG C with the speed of 6 DEG C/min, insulation 3h, vacuum tightness is 1 × 10
-3pa; Sinter complete, vacuum tightness is 1 × 10
-4pa ~ 1 × 10
-3pa; 1250 DEG C are cooled to, insulation 1h with the speed of 15 DEG C/min; 800 DEG C are cooled to, insulation 1.5h, then furnace cooling with the speed of 13 DEG C/min; The obtained complete three-dimensional communication of porous tantalum medical embedded material hole, it is 5.31g/cm that contriver records its density by standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001
3, porosity is about 70%, ultimate compression strength 65.2MPa, flexural strength 73.8MPa, Young's modulus 2.6GPa.
Embodiment 2
A kind of preparation method of porous tantalum medical embedded material, be that the pure tantalum powder of 10 μm is transported on the platform of 3 D-printing by particle diameter, roll extrusion laying, designing the sample size that will prepare is φ 10 × 100mm, and by its UG file molding equipment, it is shaping to carry out selective laser sintering.Computer controls the two-dimensional scan track of laser beam according to the hierarchical model of prototype, sinter the pure tantalum powder of conveying selectively to form an aspect of part, after powder completes one deck, working piston declines 50 μm, paving powder system spreads new tantalum powder, controls laser beam and scans the new layer of sintering again, so move in circles, be layering, until three-dimensional samples is shaping; In selective laser sintering process, laser power is at 65W, and sweep velocity is 15mm/s, and sweep span is 0.1mm, and every layer spreads bisque thick is 70 μm, and whole moulding process is carried out in argon atmosphere, and purity of argon is greater than 99.999%.Then take out molded samples, put into vacuum oven and carry out high-temperature vacuum sintering, rise to 1250 DEG C with the speed of 13 DEG C/min from room temperature, insulation 0.5h, vacuum tightness is 1 × 10
-4pa; Rise to 1500 DEG C with the speed of 20 DEG C/min, insulation 0.5h, vacuum tightness is 1 × 10
-4pa ~ 1 × 10
-3pa; Rise to 2200 DEG C with the speed of 20 DEG C/min, insulation 240min, vacuum tightness is 1 × 10
-3pa; Sinter complete, vacuum tightness is 1 × 10
-4pa ~ 1 × 10
-3pa; 1550 DEG C are cooled to, insulation 1h with the speed of 15 DEG C/min; Be cooled to 1200 DEG C with the speed of 18 DEG C/min, insulation 1.5h, is cooled to 800 DEG C with the speed of 12 DEG C/min, then furnace cooling; The obtained complete three-dimensional communication of porous tantalum medical embedded material hole, it is 5.82g/cm that contriver records its density by standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001
3, porosity is about 65%, ultimate compression strength 70.5MPa, flexural strength 82.3MPa, Young's modulus 3.3GPa.
Embodiment 3 ~ 7: according to the following steps and processing parameter carry out, all the other are with embodiment 1.
Gained porous tantalum finished product three-dimensional is communicated with completely, porous nickel distribution, and good biocompatibility is as follows by preceding method detected result:
| Embodiment | 3 | 4 | 5 | 6 | 7 |
| Density (g/cm 3) | 5.37 | 5.63 | 7.00 | 6.25 | 5.88 |
| Porosity (%) | 80 | 75 | 60 | 68 | 70 |
| Young's modulus (GPa) | 5.5 | 3.5 | 6.5 | 5.0 | 6.1 |
| Flexural strength (MPa) | 135 | 102 | 127 | 130 | 143 |
| Ultimate compression strength (MPa) | 85 | 72 | 80 | 90 | 83 |
Claims (1)
1. the preparation method of a porous tantalum medical embedded material, be that the pure tantalum powder of 10 μm is transported on the platform of 3 D-printing by particle diameter, roll extrusion laying, designing the sample size that will prepare is φ 10 × 100mm, and by its UG file molding equipment, it is shaping to carry out selective laser sintering; Computer controls the two-dimensional scan track of laser beam according to the hierarchical model of prototype, sinter the pure tantalum powder of conveying selectively to form an aspect of part, after powder completes one deck, working piston declines 50 μm, paving powder system spreads new tantalum powder, controls laser beam and scans the new layer of sintering again, so move in circles, be layering, until three-dimensional samples is shaping; In selective laser sintering process, laser power is at 58W, and sweep velocity is 19mm/s, and sweep span is 0.13mm, and every layer spreads bisque thick is 80 μm, and whole moulding process is carried out in argon atmosphere, and purity of argon is greater than 99.999%; Then take out molded samples, put into vacuum oven and carry out high-temperature vacuum sintering, the speed of 17 DEG C/min rises to 1750 DEG C from room temperature, and insulation 135min, be chilled to 260 DEG C with stove, vacuum tightness is 10
-4pa; 1650 DEG C are risen to, insulation 220min with the speed of 15 DEG C/min; Rise to 2150 DEG C with the speed of 7.5 DEG C/min, insulation 160min, vacuum tightness is 10
-3pa; Vacuum tightness is 10
-4pa ~ 10
-3pa; 1520 DEG C are cooled to, insulation 45min with the speed of 15 DEG C/min; 1220 DEG C are cooled to, insulation 60min with the speed of 16 DEG C/min; 800 DEG C are cooled to, then furnace cooling with the speed of 13 DEG C/min; Sinter complete, vacuum tightness is 10
-4pa ~ 10
-3pa, is warming up to 850 DEG C, insulation 420min with 20 DEG C/min, then is chilled to 400 DEG C, insulation 270min with 4 DEG C/min, then cools to room temperature with the furnace.
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| CN106390198B (en) * | 2016-09-19 | 2019-07-23 | 西安交通大学 | A kind of forming of precinct laser and electroreduction prepare personalized porous implant method |
| CN107598166B (en) * | 2017-09-13 | 2020-01-24 | 西安赛隆金属材料有限责任公司 | Method for preparing porous tantalum medical implant material based on electron beam selective melting technology |
| CN107901419B (en) * | 2017-12-21 | 2019-09-27 | 北京工业大学 | A method of annealing regulation PA3200 3D printing surface of shaped parts wetability |
| KR102115225B1 (en) * | 2018-06-20 | 2020-05-27 | 한국생산기술연구원 | One-step manufacturing method of laminated molding porous component |
| CN109261970B (en) * | 2018-10-23 | 2020-10-16 | 武汉三迪创为科技有限公司 | 3D printing equipment and method for preparing medical porous tantalum metal implant material by using same |
| CN109513050B (en) * | 2018-12-17 | 2021-08-17 | 广东省新材料研究所 | Gradient porous structure personalized tantalum implant and preparation method and application thereof |
| CN110421172A (en) * | 2019-08-27 | 2019-11-08 | 西安九洲生物材料有限公司 | A method of medical porous tantalum part is prepared based on selective laser melting process |
| CN111299584B (en) * | 2019-12-17 | 2021-05-25 | 吉林大学 | Preparation method of bionic impact-resistant multilayer composite gradient material based on amorphous alloy |
| CN113427022B (en) * | 2021-07-02 | 2023-09-22 | 长沙理工大学 | High-strength high-toughness post-treatment method for 3D printing biomedical metal tantalum and metal tantalum |
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| US20090051082A1 (en) * | 2006-04-13 | 2009-02-26 | Sagawa Printing Co., Ltd. | Method for producing artificial bone |
| DE102007041775B3 (en) * | 2007-09-04 | 2008-10-02 | Eads Deutschland Gmbh | Production of metal castings with foam structure uses e.g. laser to melt to melt metal wire positioned near surface of casting, foaming agent being added to molten area and process continued in controlled way to produce whole structure |
| CN101507839B (en) * | 2009-03-27 | 2012-10-10 | 陕西科技大学 | Preparation method of bionic human bone biologic material |
| CN101709419B (en) * | 2009-12-18 | 2011-09-28 | 北京有色金属研究总院 | Tantalum foam and preparation method thereof |
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