CN104646669A - Biomedical porous pure-titanium implant material and preparation method thereof - Google Patents

Biomedical porous pure-titanium implant material and preparation method thereof Download PDF

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Publication number
CN104646669A
CN104646669A CN201310603135.2A CN201310603135A CN104646669A CN 104646669 A CN104646669 A CN 104646669A CN 201310603135 A CN201310603135 A CN 201310603135A CN 104646669 A CN104646669 A CN 104646669A
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embedded
powder
pure titanium
tetrakaidecahedron
porous pure
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CN201310603135.2A
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Chinese (zh)
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陈贤帅
李子夫
戚留举
张春雨
孙学通
马得贵
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广州中国科学院先进技术研究所
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Publication of CN104646669A publication Critical patent/CN104646669A/en

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Abstract

The invention discloses a preparation method of a biomedical porous pure-titanium implant material. The method comprises the steps of S1, constructing a three-dimensional model of the implant material through drawing software, slicing through layering software, conveying the obtained two-dimensional section information to a computer control system of an SLM former, and providing a laser scanning route; S2, paving a layer of titanium powder being 30 to 70 microns in thickness on a workbench of the SLM former through a powder paving layer; S3, performing selective laser meting for the titanium powder through a laser beam under the conditions that the power is 90 to 100W, the scanning spacing is 0.10 to 0.20mm, and the scanning speed is 275 to 540mm/s to obtain a layer of sections of the implant material, and synchronously lowering down the worktable in a distance equal to the height of a layer of powder; S4, repeating the steps 2 and 3 until the three-dimensional model of the implant material is formed; S5, automatically stopping working by the SLM former, cooling the three-dimensional model to reach room temperature, then performing sand blasting to obtain the porous pure-titanium implant material; the three-dimensional model is a porous structural mode using a tetrakaidecahedron unit as a dot matrix and formed by repeatedly accumulating the tetrakaidecahedron units.

Description

Bio-medical porous pure titanium embedded material and preparation method thereof

Technical field

The present invention relates to a kind of 3D printing technique, specifically, relate to a kind of bio-medical porous embedded material and preparation method thereof.

Background technology

3D prints (3Dprinting), the i.e. one of rapid shaping technique, and it is a kind of based on mathematical model file, uses powdery metal or plastics etc. can jointing material, is carried out the technology of constructed object by the mode successively printed.3D prints and normally adopts digital technology file printing machine to realize.Past, its field such as Making mold, industrial design of being everlasting was used to modeling, existing just gradually for the direct manufacture of some products, had had the parts using this technology to print.This technology is at jewelry, footwear, industrial design, building, engineering and construction (AEC), automobile, and Aero-Space, dentistry and medical industries, education, GIS-Geographic Information System, civil engineering, gun and other field are applied all to some extent.

In recent years, along with growth in the living standard, the mankind have entered the aging stage, human body hard tissue generation pathology or to sustain damage be ubiquitous problem, usually need the sclerous tissues replacing or repair pathology or damage by performing the operation.Traditional bone alternate material all adopts fine and close metal or alloy, as cobalt-base alloys, stainless steel, titanium-base alloy etc. can be used for hip replacement.With people's bone photo ratio of loose structure, these alloys have high-intensity high-tenacity and high elastic modulus, can produce stress shielding after implantation, thus cause implant and people's synosteosis to occur to loosen, and occur local bone absorbing phenomenon.

Wherein, relative to other metals, the advantages such as titanium or titanium alloy has density little (close to people's bone), specific strength is high, elastic modelling quantity is lower, rotproofness is good, biocompatibility is excellent, are widely used.But titanium or titanium alloy does not still mate with the elastic modelling quantity of bone.For solving the problem, in medical metal material, introduce hole, by adjusting the shape of hole and size, porosity and three-dimensional connectivity to reach the mechanical property of mating with bone photo.In addition, loose structure is conducive to osteoblastic growth, promotes that new bone tissue is rebuild, and making implant with forming three dimensional biological locking between bone, improving the steadiness of the former implant.

At present, the conventional method preparing bio-medical porous material comprises powder metallurgic method, metaliding, gel injection-moulding method, combustion synthesis method.These traditional methods existing cannot realize controlling the precise forming of pore shape, pore size, porosity and hole three-dimensional connectivity--and controllable precise is shaping, then cannot be shaping for very complicated structure.

Follow-up, develop again selective laser sintering (Selective Laser Sintering, SLS) legal system for porous material.Existing a kind of selective laser sintering prepares the method for biological stephanoporate stainless steel embedded material, first adopts method with plastic film to prepare the coated 316L powder of stainless steel of thermoplastic polymer; Then adopt Selective Laser Sintering shaping coating film metal powder, obtain preform; The metal implant material of porous is obtained finally by thermal debinding and double sintering.Selective Laser Sintering (SLS) is though can prepare complex porous structure, and hole precision is accurate not, and needs the subsequent treatment such as metallic cementation, and flow process is complicated.

Summary of the invention

The object of the present invention is to provide a kind of preparation method of bio-medical porous pure titanium embedded material, solve in prior art the hole precision preparing complex porous structure existence accurate not, and need the subsequent treatment such as metallic cementation, the problem of flow process complexity, more accurately can control the forming dimension of loose structure, realize the one-shot forming of loose structure.

Another object of the present invention is to provide a kind of density and the high bio-medical porous pure titanium embedded material of mechanical property, after implant into body, its loose structure is conducive to osteoblastic growth, promotes that new bone tissue is rebuild, improves the steadiness of embedded material.

To achieve these goals, the technical solution adopted in the present invention is as follows:

A preparation method for bio-medical porous pure titanium embedded material, comprises the following steps:

S1, employing mapping software build the threedimensional model of embedded material, and carried out slicing treatment by delamination software, the computer control system of SLM forming machine is transported to, to provide machining path during laser scanning after the two-dimensional section information obtained being preserved with SLM form;

S2, employing power spreading device lay a layer thickness on the workbench of SLM forming machine are the titanium powder of 30 ~ 70 μm, and workbench is provided with a substrate, adjust the levelness of substrate and substrate is carried out preheating, do not need preheating during next paving powder before first paving powder;

S3, laser beam carry out to titanium powder the layer cross section that selective laser melting obtains embedded material with the sweep speed of 90 ~ 100W power, 0.10 ~ 0.20mm sweep span and 275 ~ 540mm/s under the guidance of computer control system, and simultaneously workbench declines the height of one deck powder;

S4, repetition step S2 and step S3, until scanned last layer cross section of model, the threedimensional model of embedded material is shaping;

S5, SLM forming machine quits work automatically, after threedimensional model is cooled to room temperature, in SLM forming machine, takes out substrate, takes off threedimensional model and do blasting treatment from substrate, namely obtain porous pure titanium implant material;

Wherein, the loose structure model that described threedimensional model is is dot matrix with tetrakaidecahedron unit, described threedimensional model repeats accumulation by described tetrakaidecahedron unit and forms.

Further, the arm footpath of described tetrakaidecahedron unit is 400 μm, and aperture is 1000 μm, and the length of side is 810 μm.

Further, the thickness of described substrate is 0.5-1mm.

Further, the compensating factor of described laser beam is 0-40um.

Further, in step S2, in the cavity of SLM forming machine, be filled with argon gas as protective gas.

Further, in step S2, in the cavity of SLM forming machine, the concentration of oxygen is lower than 0.1%.

A kind of bio-medical porous pure titanium embedded material, comprise embedded material body, described embedded material body adopts selective laser melting technology of metal powder to make, described metal dust is pure titanium powder, the loose structure that described embedded material body is is dot matrix with tetrakaidecahedron unit, described embedded material body repeats accumulation by described tetrakaidecahedron unit and forms, and the arm footpath of described tetrakaidecahedron unit is 400 μm, aperture is 1000 μm, and the length of side is 810 μm.

Compared with prior art, the present invention proposes novel bio-compatible loose structure design, can to the shape of loose structure hole, spatial distribution, size accurately controls, integration system is for complex porous structure, do not need subsequent heat treatment or metallic cementation, flow process is simple, hole precision is accurate, and obtained porous pure titanium implant material density and mechanical property high, after implant into body, its loose structure is conducive to osteoblastic growth, promote that new bone tissue is rebuild, make porous pure titanium implant material with forming three dimensional biological locking between bone, improve the steadiness of porous pure titanium implant material, meet the various demands of human body to embedded material.

Accompanying drawing explanation

Fig. 1 is the model schematic of tetrakaidecahedron cellular construction of the present invention;

Fig. 2 is the loose structure model schematic being dot matrix with tetrakaidecahedron cellular construction of the present invention;

Fig. 3 is process flow diagram of the present invention.

Detailed description of the invention

Below in conjunction with the drawings and specific embodiments, bio-medical porous pure titanium embedded material of the present invention and preparation method thereof is described further.

Selective laser melting technology (Selective Laser Melting) is advanced increasing material manufacturing technology, it does not need mould, " piled up layer by layer " by dusty material, melt the principle of every layer of powder completely, by computer-aided design data model, produce the controllable precise manufacture of complicated three-dimensional entity model fast.

Refer to Fig. 1, Fig. 2 and Fig. 3, the invention discloses a kind of preparation method of bio-medical porous pure titanium embedded material, comprise the following steps:

S1, employing mapping software build the threedimensional model of embedded material, and carried out slicing treatment by delamination software, the computer control system of SLM forming machine is transported to, to provide machining path during laser scanning after the two-dimensional section information obtained being preserved with SLM form.

Described mapping software can be the engineering drawing software such as CAD, Solidworks, UG, ProE, according to the required practical structures preparing embedded material, design and set up the threedimensional model of actual loose structure, and save as STL form, then import in Autofab software and layered shaping is carried out to threedimensional model, and set machined parameters, preserve and derive the computer control system of file to SLM forming machine of SLM form.

Refer to Fig. 1 and Fig. 2, the loose structure model that threedimensional model of the present invention is is dot matrix with tetrakaidecahedron unit, described threedimensional model repeats accumulation by described tetrakaidecahedron unit and forms, and the arm footpath of described tetrakaidecahedron unit is 400 μm, aperture is 1000 μm, and the length of side is 810 μm.Particularly, described machined parameters comprises the power of laser, sweep span, sweep speed and compensating factor.In the present invention, the scan power of setting laser is 90 ~ 100W, and sweep span is 0.10 ~ 0.20mm, and sweep speed is 275 ~ 540mm/s, and the light-dark cycle factor is set as 0-40um.

S2, employing power spreading device lay a layer thickness on the workbench of SLM forming machine are the titanium powder of 30 ~ 70 μm, and workbench is provided with a substrate, adjust the levelness of substrate and substrate is carried out preheating, do not need preheating during next paving powder before first paving powder.

Refer to Fig. 2, the workbench of SLM forming machine is provided with the thick substrate of 0.5-1mm, described substrate provides heat radiation and stressed support in the forming process of threedimensional model.The substrate increased in the bottom of threedimensional model is too thin or too thick, can affect the Forming Quality of described threedimensional model, makes described three-dimensional model deformation.Preferably, the thick substrate of 0.5mm is increased in the bottom of threedimensional model.

Before laser beam scans; first adjust the processing environment in SLM forming machine cavity, in the cavity of SLM forming machine, be filled with argon gas as protective gas, in the cavity of SLM forming machine, the concentration of oxygen is lower than 0.1%; to avoid titanium valve to be oxidized, affect the preparation of described porous pure titanium implant material.On the workbench of SLM forming machine, the titanium powder thickness of lay is 30 ~ 70 μm, and the too thin meeting of thickness of titanium powder scans substrate, easily causes substrate to melt, and makes the porous pure titanium implant material obtained occur uneven; The too thick meeting of thickness of titanium powder makes the poor connectivity between itself and substrate.The limiting temperature of SLM forming machine is 200 DEG C, usually before first paving powder, first adjusts the levelness of substrate, base plate heating is to 150-200 DEG C of preheating 20-30 minute again, preferably, by base plate heating to 200 DEG C preheating 25 minutes, when adopting next time power spreading device to carry out paving powder, substrate does not carry out preheating.

S3, laser beam carry out to titanium powder the layer cross section that selective laser melting obtains embedded material with the sweep speed of 90 ~ 100W power, 0.10 ~ 0.20mm sweep span and 275 ~ 540mm/s under the guidance of computer control system, and simultaneously workbench declines the height of one deck powder.

Laser beam scans with the sweep speed of 90 ~ 100W power, 0.10 ~ 0.20mm sweep span and 275 ~ 540mm/s, the power of laser beam is too low, and the density of obtained described porous pure titanium implant material is poor, and the power of laser beam flying is too high, sweep speed is too fast, and energy is low.Preferably, the sweep span of laser beam is 0.13mm.

S4, repetition step S2 and step S3, until scanned last layer cross section of model, the threedimensional model of embedded material is shaping.

The thickness 30 ~ 70 μm of the first decline one deck too powder of the workbench of SLM forming machine, and then lay a layer thickness is the titanium powder of 30 ~ 70 μm on the substrate adopting power spreading device to arrange on the workbench of SLM forming machine, then laser beam carries out to titanium powder the layer cross section that selective laser melting obtains embedded material with the sweep speed of 90 ~ 100W power, 0.10 ~ 0.20mm sweep span and 275 ~ 540mm/s under the guidance of computer control system, simultaneously workbench declines the height of one deck powder, and circulation paving powder and scanning are until threedimensional model is shaping.

S5, SLM forming machine quits work automatically, after threedimensional model is cooled to room temperature, in SLM forming machine, takes out substrate, takes off threedimensional model and do blasting treatment from substrate, namely obtain porous pure titanium implant material.

Through density and compression test test, what the present invention designed is 400 μm with arm footpath, aperture is 1000 μm, the tetrakaidecahedron loose structure model of the length of side to be 810 μm of tetrakaidecahedron unit be dot matrix, by the porous pure titanium implant material that above-mentioned processing step is obtained, suffered maximum stress is 372.24Mpa, lower than the yield strength 559Mpa of titanium, elastic modelling quantity is 8.34Gpa, yield strength is 278.86Mpa, be 1 ~ 10Gpa with the elastic modelling quantity of cancellous bone, compression strength is that 2 ~ 200Mpa matches, mechanical property meets the basic demand of body implant's material, it is a kind of desirable porous metals implant material.

Refer to Fig. 1, Fig. 2 and Fig. 3, the invention also discloses a kind of bio-medical porous pure titanium embedded material, described bio-medical porous pure titanium embedded material comprises embedded material body, described embedded material body adopts selective laser melting technology of metal powder to make, and described metal dust is pure titanium powder.Described embedded material body of stating is the loose structure that is dot matrix with tetrakaidecahedron unit, and described embedded material body repeats accumulation by described tetrakaidecahedron unit and forms, and the arm footpath of described tetrakaidecahedron unit is 400 μm, and aperture is 1000 μm, and the length of side is 810 μm.After described bio-medical porous pure titanium embedded material implant into body, its loose structure is conducive to osteoblastic growth, promote that new bone tissue is rebuild, making described bio-medical porous pure titanium embedded material with forming three dimensional biological locking between bone, improving the steadiness of described bio-medical porous pure titanium embedded material.

The process that employing selective laser melting technology of metal powder prepares described embedded material body is as follows:

S1, employing mapping software build the threedimensional model of embedded material, and carried out slicing treatment by delamination software, the computer control system of SLM forming machine is transported to, to provide machining path during laser scanning after the two-dimensional section information obtained being preserved with SLM form.

S2, employing power spreading device lay a layer thickness on the workbench of SLM forming machine are the titanium powder of 30 ~ 70 μm, and workbench is provided with a substrate, adjust the levelness of substrate and substrate is carried out preheating, do not need preheating during next paving powder before first paving powder.

S3, laser beam carry out to titanium powder the layer cross section that selective laser melting obtains embedded material with the sweep speed of 90 ~ 100W power, 0.10 ~ 0.20mm sweep span and 275 ~ 540mm/s under the guidance of computer control system, and simultaneously workbench declines the height of one deck powder.

S4, repetition step S2 and step S3, until scanned last layer cross section of model, the threedimensional model of embedded material is shaping.

S5, SLM forming machine quits work automatically, after threedimensional model is cooled to room temperature, in SLM forming machine, takes out substrate, takes off threedimensional model and do blasting treatment from substrate, namely obtains described embedded material body.

The present invention proposes novel bio-compatible loose structure design, solve problem prepared by complex porous structure, accurately can control the shape of loose structure hole, spatial distribution, size, integration system is for complex porous structure, do not need subsequent heat treatment or metallic cementation, flow process is simple, and hole precision is accurate, and obtained porous pure titanium implant material density and mechanical property high, meet the various demands of human body to embedded material.

Above-mentioned explanation is the detailed description for the better possible embodiments of the present invention, but embodiment is also not used to limit patent claim of the present invention, the equal change completed under all disclosed technical spirits or modification are changed, and all should belong to the present invention and contain the scope of the claims.

Claims (7)

1. a preparation method for bio-medical porous pure titanium embedded material, is characterized in that, comprise the following steps:
S1, employing mapping software build the threedimensional model of embedded material, and carried out slicing treatment by delamination software, the computer control system of SLM forming machine is transported to, to provide machining path during laser scanning after the two-dimensional section information obtained being preserved with SLM form;
S2, employing power spreading device lay a layer thickness on the workbench of SLM forming machine are the titanium powder of 30 ~ 70 μm, and workbench is provided with a substrate, adjust the levelness of substrate and substrate is carried out preheating, do not need preheating during next paving powder before first paving powder;
S3, laser beam carry out to titanium powder the layer cross section that selective laser melting obtains embedded material with the sweep speed of 90 ~ 100W power, 0.10 ~ 0.20mm sweep span and 275 ~ 540mm/s under the guidance of computer control system, and simultaneously workbench declines the height of one deck powder;
S4, repetition step S2 and step S3, until scanned last layer cross section of model, the threedimensional model of embedded material is shaping;
S5, SLM forming machine quits work automatically, after threedimensional model is cooled to room temperature, in SLM forming machine, takes out substrate, takes off threedimensional model and do blasting treatment from substrate, namely obtain porous pure titanium implant material;
Wherein, the loose structure model that described threedimensional model is is dot matrix with tetrakaidecahedron unit, described threedimensional model repeats accumulation by described tetrakaidecahedron unit and forms.
2. the preparation method of bio-medical porous pure titanium embedded material as claimed in claim 1, is characterized in that: the arm footpath of described tetrakaidecahedron unit is 400 μm, and aperture is 1000 μm, and the length of side is 810 μm.
3. the preparation method of bio-medical porous pure titanium embedded material as claimed in claim 1, is characterized in that: the thickness of described substrate is 0.5-1mm.
4. the preparation method of bio-medical porous pure titanium embedded material as claimed in claim 1, is characterized in that: the compensating factor of described laser beam is 0-40um.
5. the preparation method of bio-medical porous pure titanium embedded material as claimed in claim 1, is characterized in that: in step S2, is filled with argon gas as protective gas in the cavity of SLM forming machine.
6. the preparation method of bio-medical porous pure titanium embedded material as claimed in claim 1, it is characterized in that: in step S2, in the cavity of SLM forming machine, the concentration of oxygen is lower than 0.1%.
7. a bio-medical porous pure titanium embedded material, comprise embedded material body, it is characterized in that: described embedded material body adopts selective laser melting technology of metal powder to make, described metal dust is pure titanium powder, the loose structure that described embedded material body is is dot matrix with tetrakaidecahedron unit, described embedded material body repeats accumulation by described tetrakaidecahedron unit and forms, and the arm footpath of described tetrakaidecahedron unit is 400 μm, aperture is 1000 μm, and the length of side is 810 μm.
CN201310603135.2A 2013-11-25 2013-11-25 Biomedical porous pure-titanium implant material and preparation method thereof CN104646669A (en)

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CN104985183A (en) * 2015-06-12 2015-10-21 华南协同创新研究院 Low-elasticity-modulus titanium-based jawbone implant and preparation method thereof
CN105256160A (en) * 2015-10-29 2016-01-20 广州有色金属研究院 3D printing method for ceramic-based nickel alloy composite material
CN105397087A (en) * 2015-10-29 2016-03-16 西安铂力特激光成形技术有限公司 Selective laser melting and forming method for TC4 titanium alloy hollowed-out artificial bone
CN105496611A (en) * 2015-12-15 2016-04-20 广州中国科学院先进技术研究所 Porous implant filled with O-intersecting lines units
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CN107790719A (en) * 2017-11-13 2018-03-13 成都优材科技有限公司 Based on selective laser molten metal fine cellular structure forming method
CN107952962A (en) * 2017-11-20 2018-04-24 淮阴工学院 A kind of functionally gradient biomimetic features titanium alloy artificial implant and its manufacturing process
CN108213427A (en) * 2018-01-10 2018-06-29 南方科技大学 A kind of high-performance titanium material fabrication process
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CN108580851A (en) * 2018-05-14 2018-09-28 重庆大学 A kind of preparation method for the MgTi compound castings that combination interface is strengthened
CN109396436A (en) * 2018-12-04 2019-03-01 陕西理工大学 A kind of pure titanium 3D printing increasing material manufacturing method
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CN106148749A (en) * 2015-04-09 2016-11-23 中国科学院金属研究所 One has high intensity and the high-selenium corn gradient porous Ti-6Al-4V block materials of energy and preparation method thereof concurrently
CN104985183B (en) * 2015-06-12 2017-10-24 华南协同创新研究院 A kind of low elastic modulus titanium-based jawbone implant and preparation method thereof
CN104985183A (en) * 2015-06-12 2015-10-21 华南协同创新研究院 Low-elasticity-modulus titanium-based jawbone implant and preparation method thereof
CN105256160A (en) * 2015-10-29 2016-01-20 广州有色金属研究院 3D printing method for ceramic-based nickel alloy composite material
CN105397087A (en) * 2015-10-29 2016-03-16 西安铂力特激光成形技术有限公司 Selective laser melting and forming method for TC4 titanium alloy hollowed-out artificial bone
CN105559947A (en) * 2015-12-15 2016-05-11 广州中国科学院先进技术研究所 Preparation method of porous implant filled with O-intersecting lines units
CN105496611A (en) * 2015-12-15 2016-04-20 广州中国科学院先进技术研究所 Porous implant filled with O-intersecting lines units
CN105944146A (en) * 2016-04-25 2016-09-21 东莞理工学院 Preparation method of biomedical porous magnesium bone tissue engineering scaffold
CN106247159A (en) * 2016-08-02 2016-12-21 西安铂力特激光成形技术有限公司 A kind of hollow-out unit body printed for metal 3D and the part with this cell cube
CN107790719A (en) * 2017-11-13 2018-03-13 成都优材科技有限公司 Based on selective laser molten metal fine cellular structure forming method
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CN108580851A (en) * 2018-05-14 2018-09-28 重庆大学 A kind of preparation method for the MgTi compound castings that combination interface is strengthened
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