CN105797206A - Biomedical composite implant material and preparing method thereof - Google Patents

Biomedical composite implant material and preparing method thereof Download PDF

Info

Publication number
CN105797206A
CN105797206A CN201610141352.8A CN201610141352A CN105797206A CN 105797206 A CN105797206 A CN 105797206A CN 201610141352 A CN201610141352 A CN 201610141352A CN 105797206 A CN105797206 A CN 105797206A
Authority
CN
China
Prior art keywords
composite
powder
implant
bio
ball
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610141352.8A
Other languages
Chinese (zh)
Other versions
CN105797206B (en
Inventor
陈悦昶
郑增
朱俊
韩李松
王士学
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui top technology Co., Ltd.
Original Assignee
Shanghai Tuobao Electromechanical Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Tuobao Electromechanical Technology Co Ltd filed Critical Shanghai Tuobao Electromechanical Technology Co Ltd
Priority to CN201610141352.8A priority Critical patent/CN105797206B/en
Priority to PCT/CN2016/086964 priority patent/WO2017152541A1/en
Publication of CN105797206A publication Critical patent/CN105797206A/en
Application granted granted Critical
Publication of CN105797206B publication Critical patent/CN105797206B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/025Other specific inorganic materials not covered by A61L27/04 - A61L27/12
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20Direct sintering or melting
    • B22F10/28Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30Process control
    • B22F10/36Process control of energy beam parameters
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30Process control
    • B22F10/36Process control of energy beam parameters
    • B22F10/366Scanning parameters, e.g. hatch distance or scanning strategy
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/66Treatment of workpieces or articles after build-up by mechanical means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/02Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30Process control
    • B22F10/32Process control of the atmosphere, e.g. composition or pressure in a building chamber
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30Process control
    • B22F10/36Process control of energy beam parameters
    • B22F10/362Process control of energy beam parameters for preheating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Automation & Control Theory (AREA)
  • Physics & Mathematics (AREA)
  • Medicinal Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dermatology (AREA)
  • Plasma & Fusion (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Inorganic Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Optics & Photonics (AREA)
  • Mechanical Engineering (AREA)
  • Prostheses (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention provides a composite material. The composite material is prepared from, by volume, 85-95% of stainless steel powder and 5-15% of calcium silicate powder. The invention further provides application of the composite material as a biomedical composite implant material and a preparing method thereof. According to the preparing method of the biomedical composite implant material, after the components are mixed, the stirring and ball milling technology is adopted for preparing composite powder; after a human body implant three-dimensional model is constructed, the slicing technology is adopted for calculating the two-dimensional cross section, the composite powder is laid, scanned through laser beams and melted to form one two-dimensional cross section of an implant, and the steps are repeated, so that the implant body three-dimensional model is formed and subjected to after-treatment to obtain the biomedical composite implant material. According to the biomedical composite implant material and the preparing method thereof, mechanical properties and biocompatibility of the material can be controlled effectively, and various requirements of the human body for the implant material can be met.

Description

A kind of bio-medical composite implantation material and preparation method thereof
Technical field
The invention belongs to biology medical material technical field, relate to a kind of bio-medical composite implantation material and preparation method thereof, tool Body relates to a kind of employing stirring ball-milling and selective laser melting technology quickly prepares bio-medical 316L rustless steel with calcium silicates again Close embedded material and method thereof.
Background technology
Selective laser melting technology is that a kind of new pattern laser increases material manufacturing technology, and principle based on layering superposition is swashed by high energy Light beam is completely melt metal dust, thus the 3 D auto realizing part shapes.This technology is a rapid melting and the mistake of solidification Journey, formation of parts crystal grain is tiny, high comprehensive performance, has significant advantage in terms of shaping fine labyrinth.Additionally, base Yu Zengcai manufactures and the feature of dusty material, and selective laser melting technology also has the advantage saving material.Based on above advantage, This technology has been applied to multiple fields such as Aero-Space, biological manufacture and military project.Especially at biological manufacture view, this technology because of Its high accuracy, high customization and can shape the feature of complex internal structure, be extremely suitable for the manufacture of human bearing's body.
Bio-medical material refers to for organism diagnoses, treats, repairs or replaces disease damage tissue, organ, or promotes The material of its function.In hard tissue repair and replacement field, whole world biomaterial industry amount of production is annual the most quickly to be increased. According to estimates, 300,000 example joint replacement surgery will be carried out every year in the U.S.;The whole world accepts hipbone operation every year then has 500,000 people left The right side, and this numeral is also increasing with the speed of 100,000 person/year.But only in Britain, the hipbone carried out every year replaces in operation Just having 18% is to reprocess operation;In China, the most also there is millions of example Cranial defect patient, but in the clinical practice of biologic implant On, also it is limited only to Maxillary region (such as nasal bone, clavicle, cheekbone etc.), for carrying, position sclerous tissues (such as joint bone, is also the easiest Impaired position), the most also rarely have real successfully application.Therefore, the artificial hard tissue repair that structure is the most lasting and replacement biology Material has great practical significance, actively develops correlational study work imperative.
Rustless steel is to apply a class biomaterial the earliest, the most history of over half a century.At medical stainless steel material In, austenitic stainless steel is because of its good mechanical performance, corrosion resistance and cheap price, and is widely applied.Medical There is following subject matter in rustless steel: (1) case hardness is relatively low, and wearability is poor, sensitive to spot corrosion in the fluid environment of human body, And corrosion will pass through the cell reaction to electric current, the pH value of change tissue also discharges Ni, Cr, Mo etc. to human body Harmful metal ion, causes local organization allergy pain, even induces canceration;(2) elastic modelling quantity differs relatively big with people's osseous tissue, It is easily generated stress shielding, makes prosthetic loosening, produce bone resorption and atrophy phenomenon, ultimately cause implantation and lost efficacy;(3) bio-compatible Property poor, surface inactive, implant and form combination of shape and state after human body environment with body system, impact is implanted effect and is caused and plants Enter failure.
Hydroxyapatite, calcium phosphate, calcium silicates and the similar pottery close with natural bone composition becomes the ideal of skeleton implant Material.Research shows, calcium silicate powder or pottery have good biological activity and induction and deposition class bone hydroxyapatite in vitro The ability of layer, the formation of hydroxyapatite layer may advantageously facilitate bone conduction and the osteanagenesis of material, and promotes to be formed with soft/sclerous tissues Chemical bonding effect.But bioceramic mechanical property is poor, the application in load-bearing bone and large scale bone tissue restoration receives Limit.Therefore, metal material and bioceramic material are combined and prepare Biocomposite material and increasingly paid attention to by scholars, Become current study hotspot.
Summary of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide the system of a kind of bio-medical composite implantation material Preparation Method, this kind of bio-medical 316L rustless steel and the preparation method of calcium silicates composite implantation material, it is possible to solve in prior art Prepare the bottleneck of baroque implant, it is possible to more precisely control implant forming dimension, it is achieved the once one-tenth of implant Type, and have more preferable biocompatibility than simple metal implant.
Another object of the present invention is to bio-medical 316L rustless steel and the silicon providing a kind of comprehensive mechanical property close with people's bone Acid calcium composite implantation material, after implanting human body, is prevented effectively from stress shielding, prevents implant from loosening, improves implant material Stability.
For achieving the above object and other relevant purposes, the present invention provides a kind of composite, by volume percentages, including with Lower component:
Powder of stainless steel 85-95vol%;
Calcium silicates powder 5-15vol%.
Preferably, described composite, by volume percentages, including following components:
Powder of stainless steel 90vol%;
Calcium silicates powder 10vol%.
Preferably, described powder of stainless steel is 316L powder of stainless steel.
It is highly preferred that the mean diameter of described 316L powder of stainless steel is 40-60 μm.
It is further preferred that the mean diameter of described 316L powder of stainless steel is 50 μm.
Preferably, the mean diameter of described calcium silicates powder is 5-15 μm.
It is highly preferred that the mean diameter of described calcium silicates powder is 10 μm.
The present invention further provides a kind of composite purposes as bio-medical composite implantation material.
The present invention furthermore provides the preparation method of a kind of bio-medical composite implantation material, comprises the following steps:
1), after powder of stainless steel and calcium silicates powder being mixed, stirring ball-milling technique is used to prepare composite powder;
Preferably, described powder of stainless steel and calcium silicates powder, with volume percentage, addition be respectively 85-95vol% and 5-15vol%.
It is highly preferred that described powder of stainless steel and calcium silicates powder, with volume percentage, addition be respectively 90vol% and 10vol%.
Preferably, described powder of stainless steel is 316L powder of stainless steel.
It is highly preferred that the mean diameter of described 316L powder of stainless steel is 40-60 μm.
It is further preferred that the mean diameter of described 316L powder of stainless steel is 50 μm.
Preferably, the mean diameter of described calcium silicates powder is 5-15 μm.
It is highly preferred that the mean diameter of described calcium silicates powder is 10 μm.
Preferably, the ball mill that described stirring ball-milling technique uses is ground.
It is highly preferred that the mill ball used in described ball mill is sintered carbide ball, a diameter of 5 ± 0.1mm of described mill ball. The material of described sintered carbide ball is YG6 W-Co kind hard alloy.
It is highly preferred that the ball material mass ratio of the mill ball used in described ball mill and composite powder is 9-11:1.
It is further preferred that the ball material mass ratio of described mill ball and composite powder is 10:1.
It is highly preferred that the grinding condition of described ball mill is: the rotating speed of mixing arm: 200-300 rev/min;Ball-milling Time: 10-15 Hour.
2), after building body implant's threedimensional model, use slice process to calculate two-dimensional cross sectional, and two-dimensional cross sectional information is passed
Deliver to the control unit of selective laser melting former;
Preferably, described body implant's threedimensional model uses three-dimensional drawing software to build.Three-dimensional drawing software is used to carry out When building threedimensional model, needed for needing basis, prepare the practical structures of embedded material, design and set up actual threedimensional model, and will Three-dimensional model information saves as STL formatted file.
It is highly preferred that a kind of engineering drawing software that described three-dimensional drawing software is in CAD, Solidworks, UG, ProE.
Preferably, described slice process is to import in delamination software by three-dimensional model information, after delamination software step section, Calculate two-dimensional cross sectional again, and two-dimensional cross sectional information is saved as SLM formatted file.
It is highly preferred that described delamination software is Autofab software.Described Autofab software can be by three-dimensional (3D) model along certain One direction (Z axis) discrete for a series of two dimension aspect, obtain a series of two dimensional surface information, two dimensional surface thickness is controlled For 0.1-0.01mm.
Preferably, described selective laser melting former refers to according to selective laser melting technology (Selective Laser Melting) former be designed, manufactured.
Preferably, the control unit of described selective laser melting former refers to the calculating of selective laser melting former Machine control system.Those skilled in the art all understand, and the calculating process of unit controlled as described above, all can utilize prior art In computer, integrated circuit modules, PLD, other hardware or existing software module realize.
Described selective laser melting technology (Selective Laser Melting) is advanced increasing material manufacturing technology, and it need not mould Tool, " is piled up layer by layer " by dusty material, is completely melt the principle of every layer of powder, by computer-aided design data model, Quickly produce the controllable precise manufacture of the three-dimensional entity model of complexity.
3) on substrate, lay one layer of composite powder, according to the two-dimensional cross sectional information being stored in described control unit, use and swash Light beam scans corresponding transverse cross-sectional area and melts the composite powder in transverse cross-sectional area, forms two of implant Dimension cross section;
Preferably, described substrate is to use nut to be fixed on the underboarding on the workbench of selective laser melting equipment.
It is highly preferred that the specification of described substrate is 300mm × 300mm × 20mm (length × width × height).
Preferably, described substrate needs to preheat before first paving powder.Described preheating is to adjust substrate to laser focusing to click on OK.Described substrate plays the effect that part is fixed and dispelled the heat in the course of processing.
It is highly preferred that described preheating condition is: preheating temperature: 600-800 DEG C;Preheating time: 3-5min.
Preferably, described one layer of composite powder of laying on substrate, use power spreading device to lay.
It is highly preferred that described power spreading device is powder-laying roller.
Preferably, the thickness of described composite powder is 0.02 ± 0.01mm.
Preferably, described laser beam flying condition is: laser power: 120-180W;Sweep span: 0.07 ± 0.01mm;Sweep Retouch speed: 350-500mm/s.
It is highly preferred that described laser beam flying condition is: laser power 140-160W;Sweep span 0.07mm;Scanning speed: 400mm/s。
Preferably, before described laser beam is scanned, need the processing adjusting in the cavity of selective laser melting former Environment.
It is highly preferred that need to carry out evacuation in the cavity of described selective laser melting former.
It is further preferred that described evacuation uses mechanical pump to extract, vacuum is not more than-1Mpa.
It is highly preferred that be filled with high-purity argon gas as protective gas in the cavity of described selective laser melting former.Described height Pure argon concentration in cavity is not less than 99.99vol%.
It is highly preferred that the concentration of oxygen is less than 0.01vol% in the cavity of described selective laser melting former.Avoid selecting Property laser fusion former the oxidation of chamber in-vivo metal powder, affect the preparation of described implant material.
4) two-dimensional cross sectional of above-mentioned formation is declined the thickness height of one layer of composite powder;
Preferably, the thickness height of described one layer of composite powder of decline and the thickness height phase laying one layer of composite powder on substrate Deng.
It is the bench height accurately being adjusted selective laser melting equipment by servomotor that described two-dimensional cross sectional declines, and makes work The high precision of station declines, thus drives the high precision being fixed on workbench upper substrate to decline, and then makes formation on substrate The high precision of two-dimensional cross sectional declines.
It is highly preferred that the thickness height of described one layer of composite powder of decline is 0.02 ± 0.01mm.
5) step 3 is repeated) and 4), until it reaches the final two-dimensional cross sectional of described implant threedimensional model, so that planting Enter body three-dimensional models molding;
6) do blasting treatment after being cooled down by the threedimensional model of molding, obtain bio-medical composite implantation material.
Preferably, room temperature it is cooled to described in.Described room temperature is 20-25 DEG C.
Preferably, described blasting treatment uses compressed air to be power, to form high velocity spray beam by quartz sand high velocity jet to needing Surface of the work to be processed, to remove the powder residual of surface of the work.Described blasting treatment is the mode of conventional treatment model.
It addition, the present invention further provides a kind of bio-medical composite implantation material, above-mentioned preparation method prepare.
As it has been described above, the invention provides a kind of bio-medical composite implantation material and preparation method thereof, prepare a kind of biological Medical 316L stainless steel and calcium silicates composite implantation material, its implant material body uses selective laser melting composite powder trifling skill Art is made, and described composite powder uses stirring ball-milling 316L powder of stainless steel and calcium silicates powder to be prepared from.
Compared with prior art, a kind of bio-medical 316L rustless steel and the calcium silicates composite implantation material preparation side that the present invention provides Method, integration system is for biomedical implant material, it is not necessary to subsequent treatment, and flow process is simple.This kind of preparation method, solves existing There is in technology the bottleneck preparing baroque implant, it is possible to more precisely control implant forming dimension, it is achieved to material Mechanical property control effectively.Meanwhile, composite implantation material performance prepared by this kind of preparation method is close with people's bone, implants After human body, it is prevented effectively from stress shielding, prevents implant from loosening, improve the stability of implant material, and implant than simple metal Body has more preferable biocompatibility, and its biocompatibility is conducive to osteoblastic growth, meets each to implant material of human body The demand of kind.
Accompanying drawing explanation
Fig. 1 be shown as scanning speed be 400mm/s, laser power composite sample stress-strain diagram when being 120-180W Figure.
Fig. 2 be shown as scanning speed be 350-500mm/s, laser power composite sample stress-strain diagram when being 140W Figure.
Fig. 3 is shown as composite sample polarization curve under different laser scanning speed 350-500mm/s.
Fig. 4 is shown as composite sample polarization curve under different laser power 120-180W.
Detailed description of the invention
The present invention is expanded on further, it should be appreciated that these embodiments are merely to illustrate the present invention and need not below in conjunction with specific embodiment In limiting the scope of the invention.
Below by way of specific instantiation, embodiments of the present invention being described, those skilled in the art can be by disclosed by this specification Content understand other advantages and effect of the present invention easily.The present invention can also be added by the most different detailed description of the invention To implement or application, the every details in this specification can also be based on different viewpoints and application, in the essence without departing from the present invention Various modification or change is carried out under god.
It should be clear that the conventional equipment in the not concrete process equipment indicated or device all use this area in the following example or device; All force value and scope are all referring to relative pressure.
In addition, it is to be understood that the one or more method steps mentioned in the present invention do not repel before and after described combination step all right There is additive method step or additive method step can also be inserted, except as otherwise noted between these steps specifically mentioned; Should also be understood that the combination annexation between the one or more equipment/devices mentioned in the present invention is not repelled to set in described combination Other equipment/devices can also be there are before and after standby/device or can also be inserted it between these two equipment/devices specifically mentioned His equipment/device, except as otherwise noted.And, except as otherwise noted, the numbering of various method steps only differentiates various method steps Convenient tool, rather than for limit various method steps ordering or limit the enforceable scope of the present invention, its relativeness It is altered or modified, in the case of without essence change technology contents, when being also considered as the enforceable category of the present invention.
The equipment used in following example is as follows:
AXT-S series vertical lifting agitating ball mill (Jiangsu Ming Hai machinery);HRPM-II type SLM system selective laser melts Change former (Central China University of Science and Technology develops jointly) with Shanghai Spaceflight Equipment Manufacture Head Factory.
Embodiment 1
A kind of bio-medical composite implantation material of preparation, comprises the following steps:
(1) 90vol%316L powder of stainless steel and the 10vol% calcium silicates of mean diameter 10 μm of particle diameter 50 μm it are averaged Powder mixes, and uses ball mill to be ground, and the mill ball used in ball mill is sintered carbide ball, the diameter of described mill ball For 5mm, the diameter deviation≤0.1mm of mill ball.The mill ball used in described ball mill with the ratio of grinding media to material of composite powder is 10:1.The rotating speed of mixing arm is 200 revs/min, and Ball-milling Time is 10h.
(2) use CAD software to build body implant's threedimensional model, and three-dimensional model information is saved as STL formatted file. STL formatted file is imported in Autofab delamination software, after delamination software step section, then calculates two-dimensional cross sectional, And two-dimensional cross sectional information is saved as SLM formatted file.Autofab software can be discrete for a series of along Z axis by threedimensional model Two-dimentional aspect, obtain a series of two dimensional surface information, two dimensional surface thickness is controllable to 0.1-0.01mm.Again by SLM lattice Formula file is sent in the computer control system of selective laser melting former.
(3) composite powder of one layer of 0.02mm of laying on powder-laying roller substrate on the workbench of selective laser melting equipment is used End, wherein, the size of substrate is 300mm × 300mm × 20mm, and substrate uses nut to fix, and needs before first paving powder Adjusting and preheat to laser focusing point, preheating temperature is 700 DEG C, and preheating time is 4min.
(4) then, according to the two-dimensional cross sectional information being stored in computer control system, use laser beam flying corresponding Transverse cross-sectional area also melts the composite powder in transverse cross-sectional area, forms a two-dimensional cross sectional of implant.Laser beam flying bar Part is: laser power: 120-180W;Sweep span: 0.07mm;Scanning speed: 350-500mm/s.By above-mentioned formation Two-dimensional cross sectional declines the thickness height of the composite powder of one layer of 0.02mm.
(5) step (3) and (4) is repeated, until it reaches the final two-dimensional cross sectional of described implant threedimensional model, thus Make implant threedimensional model molding.Do blasting treatment after the threedimensional model of molding is cooled to room temperature, obtain that bio-medical is compound plants Enter material sample 1#.
Before the laser beam of selective laser melting equipment is scanned, need to adjust the chamber of selective laser melting former Internal processing environment.Use mechanical pump that working chamber is evacuated to-1Mpa, and be slowly introducing high-purity argon gas as protection Gas, and make the concentration of oxygen in working chamber less than 0.01%, to avoid metal powder to aoxidize, affect the system of described implant material Standby.
Embodiment 2
A kind of bio-medical composite implantation material of preparation, comprises the following steps:
(1) 85-95vol%316L powder of stainless steel and the 5-15vol% of mean diameter 5-15 μm of particle diameter 40-60 μm it are averaged Calcium silicates powder mixes, and uses ball mill to be ground, and the mill ball used in ball mill is sintered carbide ball, described mill ball A diameter of 5mm, the diameter deviation≤0.1mm of mill ball.The mill ball used in described ball mill and the ball material of composite powder Ratio is 9-11:1.The rotating speed of mixing arm is 300 revs/min, and Ball-milling Time is 15h.
(2) use Solidworks software building body implant's threedimensional model, and three-dimensional model information is saved as STL lattice Formula file.STL formatted file is imported in Autofab delamination software, after delamination software step section, then calculates two dimension Cross section, and two-dimensional cross sectional information is saved as SLM formatted file.Autofab software can be discrete along Z axis by threedimensional model For a series of two dimension aspect, obtaining a series of two dimensional surface information, two dimensional surface thickness is controllable to 0.1-0.01mm.Again SLM formatted file is sent in the computer control system of selective laser melting former.
(3) use and lay one layer of 0.02 ± 0.01mm's on powder-laying roller substrate on the workbench of selective laser melting equipment Composite powder, wherein, the size of substrate is 300mm × 300mm × 20mm, and substrate uses nut to fix, and spreads powder for the first time Front needs adjust and preheat to laser focusing point, and preheating temperature is 600-800 DEG C, and preheating time is 3-5min.
(4) then, according to the two-dimensional cross sectional information being stored in computer control system, use laser beam flying corresponding Transverse cross-sectional area also melts the composite powder in transverse cross-sectional area, forms a two-dimensional cross sectional of implant.Laser beam flying bar Part is: laser power: 120-180W;Sweep span: 0.07 ± 0.01mm;Scanning speed: 350-500mm/s.By above-mentioned The two-dimensional cross sectional formed declines the thickness height of the composite powder of one layer of 0.02 ± 0.01mm.
(5) step (3) and (4) is repeated, until it reaches the final two-dimensional cross sectional of described implant threedimensional model, thus Make implant threedimensional model molding.Do blasting treatment after the threedimensional model of molding is cooled to room temperature, obtain that bio-medical is compound plants Enter material sample 2#.
Before the laser beam of selective laser melting equipment is scanned, need to adjust the chamber of selective laser melting former Internal processing environment.Use mechanical pump that working chamber is evacuated to-1Mpa, and be slowly introducing high-purity argon gas as protection Gas, and make the concentration of oxygen in working chamber less than 0.01%, to avoid metal powder to aoxidize, affect the system of described implant material Standby.
Embodiment 3
By the bio-medical composite implantation material sample 1# of preparation in embodiment 1, measuring its density by electron density instrument is 6.25-6.89g/cm3, with skeleton density closest to.
Measuring its elastic modelling quantity by Hall element method young's elastic modulus tester again, concrete outcome is shown in Table 1.Can by table 1 Knowing, selecting laser scanning speed between 350-500mm/s, measuring the elastic modelling quantity meansigma methods obtained is 160.4-181.2GPa, With people's flexible bone modulus closest to, result shows that it meets implant material requirement.
Sample elastic modulus (Gpa) under the different laser scanning speed of table 1.
Under conditions of employing scanning speed is 400mm/s, laser power is respectively 120W, 140W, 160W, 180W, right Bio-medical composite implantation material sample 1# carries out laser beam flying, it is thus achieved that corresponding composite sample stress-strain diagram, specifically Result is shown in Fig. 1.Meanwhile, scanning speed is used to be respectively 350mm/s, 400mm/s, 450mm/s, 500mm/s, laser merit Under conditions of rate is 140W, bio-medical composite implantation material sample 1# is carried out laser beam flying, it is thus achieved that corresponding composite Sample stress-strain diagram, concrete outcome is shown in Fig. 2.According to the composite sample stress-strain diagram in Fig. 1-2, explanation is passed through Adjusting process parameter, can prepare the sample of different mechanical properties, and in this experimentation, it is thus achieved that meet human bearing The laboratory sample that bone requires.
Under conditions of using scanning speed to be respectively 350mm/s, 400mm/s, 450mm/s, 500mm/s, to bio-medical Composite implantation material sample 1# carries out laser beam flying, it is thus achieved that corresponding composite sample polarization curve, concrete outcome is shown in Fig. 3. Meanwhile, under conditions of using laser power to be respectively 120W, 140W, 160W, 180W, implant material to bio-medical is compound Material sample 1# carries out laser beam flying, it is thus achieved that corresponding composite sample polarization curve, concrete outcome is shown in Fig. 4.According to Fig. 3-4 In composite sample polarization curve, show this sample have in simulated body fluid excellence decay resistance, implant people Can effectively reduce implant corrosion probability after body, reduce poisonous plasma diffusing W,Mo probability, extend implant service life, improve Biocompatibility.
So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.Any it is familiar with this skill Above-described embodiment all can be modified under the spirit and the scope of the present invention or change by the personage of art.Therefore, such as All that in art, tool usually intellectual is completed under without departing from disclosed spirit and technological thought etc. Effect is modified or changes, and must be contained by the claim of the present invention.

Claims (10)

1. a composite, by volume percentages, including following components:
Powder of stainless steel 85-95vol%;
Calcium silicates powder 5-15vol%.
Composite the most according to claim 1, it is characterised in that described powder of stainless steel is 316L powder of stainless steel.
3. according to the arbitrary described composite of claim 1-2, as the purposes of bio-medical composite implantation material.
4. a preparation method for bio-medical composite implantation material, comprises the following steps:
1), after powder of stainless steel and calcium silicates powder being mixed, stirring ball-milling technique is used to prepare composite powder;
2), after building body implant's threedimensional model, use slice process to calculate two-dimensional cross sectional, and two-dimensional cross sectional information is passed Deliver to the control unit of selective laser melting former;
3) on substrate, lay one layer of composite powder, according to the two-dimensional cross sectional information being stored in described control unit, use and swash Light beam scans corresponding transverse cross-sectional area and melts the composite powder in transverse cross-sectional area, forms two of implant Dimension cross section;
4) two-dimensional cross sectional of above-mentioned formation is declined the thickness height of one layer of composite powder;
5) step 3 is repeated) and 4), until it reaches the final two-dimensional cross sectional of described implant threedimensional model, so that implanting Body three-dimensional models molding;
6) do blasting treatment after being cooled down by the threedimensional model of molding, obtain bio-medical composite implantation material.
The preparation method of bio-medical composite implantation material the most according to claim 4, it is characterised in that step 1) in, institute The ball mill stating the employing of stirring ball-milling technique is ground.
The preparation method of bio-medical composite implantation material the most according to claim 5, it is characterised in that described ball mill includes Any one of following condition or multinomial:
A1) mill ball used in described ball mill is sintered carbide ball;
A2) mill ball used in described ball mill is 9-11:1 with the ball material mass ratio of composite powder;
A3) grinding condition of described ball mill is: the rotating speed of mixing arm: 200-300 rev/min;Ball-milling Time: 10-15 hour.
The preparation method of bio-medical composite implantation material the most according to claim 4, it is characterised in that step 2) in, institute Stating body implant's threedimensional model uses three-dimensional drawing software to build.
The preparation method of bio-medical composite implantation material the most according to claim 4, it is characterised in that step 3) in, institute Stating laser beam flying condition is: laser power: 120-180W;Sweep span: 0.06-0.08mm;Scanning speed: 350-500mm/s。
The preparation method of bio-medical composite implantation material the most according to claim 4, it is characterised in that step 4) in, institute State the thickness height declining one layer of composite powder equal with the thickness height laying one layer of composite powder on substrate.
10. a bio-medical composite implantation material, is prepared by the preparation method as described in claim 4-9 is arbitrary.
CN201610141352.8A 2016-03-11 2016-03-11 A kind of bio-medical composite implantation material and preparation method thereof Active CN105797206B (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201610141352.8A CN105797206B (en) 2016-03-11 2016-03-11 A kind of bio-medical composite implantation material and preparation method thereof
PCT/CN2016/086964 WO2017152541A1 (en) 2016-03-11 2016-06-24 Composite biomedical implant material and preparation method therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610141352.8A CN105797206B (en) 2016-03-11 2016-03-11 A kind of bio-medical composite implantation material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN105797206A true CN105797206A (en) 2016-07-27
CN105797206B CN105797206B (en) 2019-04-09

Family

ID=56467372

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610141352.8A Active CN105797206B (en) 2016-03-11 2016-03-11 A kind of bio-medical composite implantation material and preparation method thereof

Country Status (2)

Country Link
CN (1) CN105797206B (en)
WO (1) WO2017152541A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110791681A (en) * 2019-10-29 2020-02-14 华中科技大学 Bioactive Ti-Ta-Nb alloy bone implant and forming method thereof

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113171209B (en) * 2021-04-27 2023-10-20 山东大学 Additive manufacturing nickel-titanium alloy femoral stem prosthesis and preparation method thereof
CN115074575A (en) * 2022-06-13 2022-09-20 长沙学院 High-strength high-bioactivity degradable zinc-based composite material and preparation method thereof
CN115673339B (en) * 2023-01-03 2023-04-07 西安赛隆增材技术股份有限公司 Three-dimensional manufacturing method of zirconium-niobium alloy orthopedic implant
CN117206544B (en) * 2023-11-09 2024-02-20 四川工程职业技术学院 Laser selective melting forming method for Zn-Cu-Mn-Mg alloy porous structure

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102512267A (en) * 2011-12-07 2012-06-27 上海交通大学 Bone restoration body with composite porous structure and preparation method thereof
US20140314964A1 (en) * 2013-04-18 2014-10-23 Arcam Ab Method and apparatus for additive manufacturing
CN104399978A (en) * 2014-11-27 2015-03-11 华南理工大学 3D (Three Dimensional) forming method for large-sized porous amorphous alloy part of complex shape
CN104972123A (en) * 2015-05-22 2015-10-14 上海悦瑞电子科技有限公司 3D printing method for molecular structure model and 3D printer

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8454362B2 (en) * 2006-10-16 2013-06-04 Natural Dental Implants Ag Customized dental prosthesis for periodontal- or osseointegration, and related systems and methods
CN101229587A (en) * 2008-02-20 2008-07-30 暨南大学 Biological ceramics titanium base compound material and manufacturing method thereof
CN101269238A (en) * 2008-04-24 2008-09-24 中南大学 316L toughening HA group biological function gradient material and preparation method thereof
CN102634687A (en) * 2012-04-18 2012-08-15 北京科技大学 Method for preparing stainless steel biological porous implant material by selective laser sintering
CN105014069A (en) * 2014-04-23 2015-11-04 中南大学 Magnesium alloy bone scaffold with controllable degradation rate and preparation method of magnesium alloy bone scaffold

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102512267A (en) * 2011-12-07 2012-06-27 上海交通大学 Bone restoration body with composite porous structure and preparation method thereof
US20140314964A1 (en) * 2013-04-18 2014-10-23 Arcam Ab Method and apparatus for additive manufacturing
CN104399978A (en) * 2014-11-27 2015-03-11 华南理工大学 3D (Three Dimensional) forming method for large-sized porous amorphous alloy part of complex shape
CN104972123A (en) * 2015-05-22 2015-10-14 上海悦瑞电子科技有限公司 3D printing method for molecular structure model and 3D printer

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
林红: "《口腔材料学 第2版 第1次印刷》", 31 December 2013, 北京:北京大学医学出版社 *
毛旭艳等: "3D打印生物材料的研究进展", 《济宁医学院学报》 *
胡晓熙等: "《无机材料性质及其发展研究 第1版第1次印刷》", 30 April 2015, 北京:中国水利水电出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110791681A (en) * 2019-10-29 2020-02-14 华中科技大学 Bioactive Ti-Ta-Nb alloy bone implant and forming method thereof

Also Published As

Publication number Publication date
CN105797206B (en) 2019-04-09
WO2017152541A1 (en) 2017-09-14

Similar Documents

Publication Publication Date Title
Bai et al. Additive manufacturing of customized metallic orthopedic implants: Materials, structures, and surface modifications
CN105797206A (en) Biomedical composite implant material and preparing method thereof
Zhao et al. Bionic design and 3D printing of porous titanium alloy scaffolds for bone tissue repair
Dall’Ava et al. 3D printed acetabular cups for total hip arthroplasty: a review article
Ho et al. A review on 3D printed bioimplants
Buj-Corral et al. Development of am technologies for metals in the sector of medical implants
Hao et al. Biomedical titanium alloys and their additive manufacturing
Guo et al. Biomedical applications of the powder‐based 3D printed titanium alloys: a review
CN103328016B (en) Implant for in-vivo insertion which is formed with a porous coating layer thereon
CN106312060B (en) A kind of preparation method of the low modulus medical titanium alloy 3-dimensional metal part of high-performance
CN104784760B (en) Low-elastic-modulus integrated titanium-based femoral handle and preparation method thereof
Song et al. The design and manufacturing of a titanium alloy beak for Grus japonensis using additive manufacturing
CN104646669A (en) Biomedical porous pure-titanium implant material and preparation method thereof
Syam et al. Rapid prototyping and rapid manufacturing in medicine and dentistry: This paper presents an overview of recent developments in the field of rapid prototyping and rapid manufacturing with special emphasis in medicine and dentistry
Vaiani et al. Ceramic materials for biomedical applications: an overview on properties and fabrication processes
CN108971500B (en) High-corrosion-resistance in-situ nano carbide reinforced stainless steel implant and forming method thereof
Koptyug et al. Additive manufacturing technology applications targeting practical surgery
CN106421892A (en) Titanium-based tantalum coating bio-scaffold material and preparation method thereof
Du et al. A systematic approach for making 3D-printed patient-specific implants for craniomaxillofacial reconstruction
Pesode et al. Additive manufacturing of metallic biomaterials and its biocompatibility
Banerjee et al. Emerging technologies in arthroplasty: additive manufacturing
CN105256160B (en) A kind of 3D printing method of ceramic base nickel alloy composite
CN109620475A (en) One kind being implanted into preparation based on CT data individuation porous titanium alloy shin bone
Dobrzański et al. Computer aided design in Selective Laser Sintering (SLS)–application in medicine
Sing Selective laser melting of novel titanium-tantalum alloy as orthopaedic biomaterial

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
CB03 Change of inventor or designer information
CB03 Change of inventor or designer information

Inventor after: Zong Jin

Inventor after: Guan Xianxian

Inventor after: Zhou Bingbing

Inventor after: Wang Liang

Inventor before: Chen Yuechang

Inventor before: Zheng Zeng

Inventor before: Zhu Jun

Inventor before: Han Lisong

Inventor before: Wang Shixue

TA01 Transfer of patent application right

Effective date of registration: 20170515

Address after: 201406 room 2, building 1800, Lane 1376, Xinyang Road, Shanghai, Fengxian District

Applicant after: Shanghai Kun Yao Electromechanical Technology Co. Ltd.

Address before: 201406 Shanghai City, Guang Qian Road, No. 558, room 7, building 107

Applicant before: SHANGHAI TUOBAO ELECTROMECHANICAL TECHNOLOGY CO., LTD.

TA01 Transfer of patent application right
CB03 Change of inventor or designer information
CB03 Change of inventor or designer information

Inventor after: Zong Jin

Inventor after: Zhou Bingbing

Inventor after: Wang Liang

Inventor before: Zong Jin

Inventor before: Guan Xianxian

Inventor before: Zhou Bingbing

Inventor before: Wang Liang

TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20170901

Address after: 241200 Anhui city of Wuhu province Fanchang County Economic Development Zone

Applicant after: Anhui top technology Co., Ltd.

Address before: 201406 room 2, building 1800, Lane 1376, Xinyang Road, Shanghai, Fengxian District

Applicant before: Shanghai Kun Yao Electromechanical Technology Co. Ltd.

GR01 Patent grant
GR01 Patent grant