Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
  • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
  • A61L27/02—Inorganic materials
  • A61L27/04—Metals or alloys
  • A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
  • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
  • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
  • A61L27/56—Porous materials, e.g. foams or sponges
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
  • B22F10/10—Formation of a green body
  • B22F10/14—Formation of a green body by jetting of binder onto a bed of metal powder
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
  • B22F10/30—Process control
  • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
  • B22F10/60—Treatment of workpieces or articles after build-up
  • B22F10/64—Treatment of workpieces or articles after build-up by thermal means
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
  • B22F3/10—Sintering only
  • B22F3/11—Making porous workpieces or articles
  • B22F3/1146—After-treatment maintaining the porosity
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B33—ADDITIVE MANUFACTURING TECHNOLOGY
  • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
  • B33Y10/00—Processes of additive manufacturing
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B33—ADDITIVE MANUFACTURING TECHNOLOGY
  • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
  • B33Y70/00—Materials specially adapted for additive manufacturing
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B33—ADDITIVE MANUFACTURING TECHNOLOGY
  • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
  • B33Y80/00—Products made by additive manufacturing
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C1/00—Making non-ferrous alloys
  • C22C1/08—Alloys with open or closed pores
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
  • C22C27/02—Alloys based on vanadium, niobium, or tantalum
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
  • A61L2430/00—Materials or treatment for tissue regeneration
  • A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F2301/00—Metallic composition of the powder or its coating
  • B22F2301/20—Refractory metals
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
  • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
  • B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
  • B29C64/10—Processes of additive manufacturing
  • B29C64/165—Processes of additive manufacturing using a combination of solid and fluid materials, e.g. a powder selectively bound by a liquid binder, catalyst, inhibitor or energy absorber
• • Y—GENERAL 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
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
  • Y02P10/00—Technologies related to metal processing
  • Y02P10/25—Process efficiency

Definitions

• the invention relates to the field of preparation of porous medical metal implant materials, and in particular to a method for preparing porous medical metal implant materials by three-dimensional printing and forming technology.
• Porous medical metal implant materials have important and special applications for the treatment of bone tissue trauma and femoral tissue necrosis.
• the common materials are metal stainless steel, porous metal titanium and the like.
• the porosity should be 30 ⁇ 80%, and the pores are preferably all connected and evenly distributed, or the pore portion is connected and the hook is distributed according to the need, so that Consistent with the growth of the human bone tissue, it also reduces the weight of the material itself, suitable for human implant use.
• the refractory metal ruthenium due to its excellent biocompatibility and mechanical properties, is expected to be used as a biomaterial for the treatment of bone tissue necrosis as a substitute for the traditional medical metal biomaterials described above. Since metal ruthenium is harmless to the human body, non-toxic, has no side effects, and with the rapid development of medicine at home and abroad, the understanding of sputum as a human implant material has further deepened, and the demand for porous metal ruthenium materials for human body has become More and more urgent, and the requirements are getting higher and higher. Among them, as a porous medical metal crucible, if it has a high uniform distribution of interconnected pores and physical and mechanical properties compatible with the human body, it is an important connecting member constituting material for ensuring the normal growth of new bone tissue.
• the preparation methods of the porous tantalum biomaterial mainly include a powder loose sintering method, a foam impregnation sintering method, a slurry foaming method, and the like, and all of these methods require application of a mold.
• Biological material The most important feature is the complex shape and high requirements for minute details. Therefore, high requirements are placed on the molding technology.
• the conventional molding technology cannot meet the requirements due to the limitation of the mold.
• a method for preparing a porous tantalum medical implant material characterized in that: the mixed tantalum powder mixed with the pure tantalum powder and the molding agent is sent into a printing platform of a three-dimensional printer, and the print head of the three-dimensional printer sprays the adhesive.
• the mixed tantalum powder is adhered to form a two-dimensional plane, and the workbench is lowered by 80-100 ⁇ m to perform the processing of the next layer, and layer-by-layer stacking is performed to remove the unbonded tantalum powder particles to obtain the initially formed sample, and then included Post-treatment of degreasing, vacuum sintering and cooling to obtain a porous enamel medical implant material;
• the volume ratio of the pure bismuth powder to the molding agent is 60 - 80: 20 - 40
• the molding agent is polyvinyl alcohol, stearic acid, hard And a binder having a mass concentration of 0.5 to 1.2% of ethyl ⁇ -cyanoacrylate.
• the blank obtained by the above three-dimensional printing is degreased to remove the binder and the molding agent, and then the conventional three-dimensionally connected porous ⁇ medical implant material can be obtained by conventional sintering and cooling treatment, and is consistent with the microstructure of the human bone tissue.
• the rate is 50 ° /. ⁇ 75°/.
• the porous metal implant material is biocompatible and biosafe.
• the above-mentioned post-treatment such as degreasing, sintering, etc. can be carried out by conventional post-treatment.
• the process parameters of the three-dimensional printing molding and sintering can be adjusted to control the porosity of the final porous crucible to meet different requirements, such as adjusting the corresponding process parameters.
• the three-dimensional printer used in the method of the present invention is well known, and the shape of the molded sample can be adjusted as needed.
• the use of the three-dimensional printer is to input the designed three-dimensional model file into the supporting software of the three-dimensional printing device for three-dimensional printing, which is conventional in the art. technology.
• the method of the invention has the advantages of simple equipment, high precision (50 ⁇ 80 ⁇ ), small volume, low cost, no pollution in work, fast forming speed and the like.
• the pure niobium powder has a powder particle size of 5 to 20 ⁇ m, and the molding agent is preferably stearic acid.
• the first layer is to remove the added molding agent and binder, and is raised from room temperature to 400 ° C at a rate of 1 to 5 ° C / min. , keep warm for 30 ⁇ 60min, increase from 400 °C to 600 ⁇ 800 °C at a rate of 0.5 ⁇ 1.5 °C / min, keep warm for 60 ⁇ 120min, keep the vacuum at about 10 - 3 Pa;
• the second stage high temperature vacuum In the sintering stage, increase to 1200 ⁇ 1250 °C at a rate of 10 ⁇ 15 °C / min, keep warm for 30 ⁇ 60min, vacuum degree is 10 - 4 Pa ⁇ 10 - 3 Pa; increase at a rate of 10 ⁇ 20 ° C / min to 1500 ° C, holding 30 ⁇ 60min, the degree of vacuum of 10- 4 Pa ⁇ 10- 3 Pa, at a rate of 6 ⁇ 20 ° C / min was raised to 2000 ⁇ 2200 ° C, holding 120
• the obtained porous tantalum implant material has better toughness, It is suitable as an alternative to porous body implant materials such as femur and facial strands in the body weight bearing part.
• the above sintering process is preferably carried out as follows: The degree of vacuum is 10 - 4 Pa ⁇ 10 - 3 Pa, 10 to 20 ° C / The temperature is raised to 1500 ⁇ 1800 °C, the temperature is 120 ⁇ 240min, the furnace is cooled to 200 - 300 °C, and then heated to 1500 ⁇ 1800 °C at 10 ⁇ 20 °C / min, the temperature is 180 ⁇ 240min, to 5 ⁇ 10 °C/min is heated to 2000 ⁇ 2200 °C, and the temperature is 120 ⁇ 360min.
• the above-mentioned sintering and cooling are further annealed, and the annealing step is a vacuum degree of 10 - 4 Pa - 10 - 3 Pa, heat up to 800 ⁇ 900 °C at 10 ⁇ 20 °C / min, heat insulation 240 ⁇ 480min, then cool to 400 °C at 2 ⁇ 5 °C / min, keep warm for 120 ⁇ 300min, then cool to room temperature with the furnace .
• a method of making a porous tantalum medical implant material is carried out as follows:
• the workbench Drop 80 ⁇ 100 ⁇ carry out the processing of the next layer, layer-by-layer stacking; place after molding until the binder is completely dried, remove the unbonded tantalum powder particles to obtain the initial molded sample, and then perform degreasing, vacuum sintering and After cooling and other post-treatment, a porous ⁇ medical implant material is obtained; the defatting is to remove the added molding agent and the binder, at a temperature of l ⁇ 5 ° C / min The rate is raised from room temperature to 400 ° C, kept for 30 ⁇ 60 min, raised from 400 ° C to 600 ⁇ 800 ° C at a rate of 0.5 ⁇ 1.5 ° C / min, kept for 60 ⁇ 120 min, and the vacuum is maintained at 10 - 3 Pa.
• the sintering is carried out as follows: the degree of vacuum is 10 - 4 Pa - 10 - 3 Pa, the temperature is raised to 1500 ⁇ 1800 ° C at 10 ⁇ 20 ° C / min, the temperature is maintained for 120 ⁇ 240 min, and the furnace is cooled to 200 ⁇ 300 ° C, then 10 ⁇ 20 ° C / min to 1500 ⁇ 1800 ° C, insulation 180 ⁇ 240min, 5 ⁇ 10 ° C / min to 2000 ⁇ 2200 ° C, insulation 120 ⁇ 360min; The cooling after sintering is 10 - 4 Pa ⁇ 10 - 3 Pa; the temperature is cooled to 1500 - 1600 ° C at a rate of 10 - 20 ° C / min, and the temperature is kept for 30 ⁇ 60 min; at a rate of 12 ⁇ 20 ° C / min Cooling to 1200 - 1250 ° C, holding for 60-90 min; cooling to 800 ° C at a rate of 10 ⁇ 20 ° C / min,
• the Three Dimensional Printing technology used in the molding process of the present invention is a rapid prototyping technology based on jetting, which can prepare various powder materials such as polymers, metals, ceramics, etc.
• the print head is on a thin layer of powder.
• the sprayed adhesive forms a two-dimensional plane, and is layer-by-layer stacked, and then the formed model is degreased, sintered, etc., and finally the desired sample is obtained.
• the three-dimensional printing technology combined with the three-dimensional modeling is a true meaning. Digital and precise processing, it has the advantages of high equipment (50 ⁇ 80 ⁇ ), low cost, small volume, no pollution during work and fast forming speed.
• the porous ⁇ medical implant material prepared by the preparation method of the invention has complete three-dimensional pores and good biocompatibility, and the mechanical properties are consistent with the human body-bearing bone tissue, thereby avoiding the mismatch between the porous ⁇ and the human body mechanical properties.
• the density of the porous tantalum medical implant material prepared by the invention is 5.00 ⁇ 7. 00g / cm 3 , the dispersion of the pores is high, the porosity is 60 ⁇ 70%, the pores are completely three-dimensionally connected and evenly distributed, the biological phase Capacitance is good, the pore size is about 200 ⁇ ⁇ ⁇ 300 ⁇ ⁇ ; the elastic modulus can reach 5. 5 ⁇ 6.
• the bending strength can reach 125 ⁇ 158Mpa
• the compressive strength can reach 80 ⁇ 90M P a.
• the preparation method has a single process and is easy to control; the whole preparation process is harmless, non-polluting, non-toxic and dusty, and has no side effects on the human body.
• Fig. 1 is a vertical microscopic analysis of the microstructure of a porous crucible prepared by the preparation method of the present invention; it can be observed from the drawing that the pores of the porous crucible obtained by the present invention are completely three-dimensionally connected and uniformly distributed.
• a method for preparing a porous tantalum medical implant material firstly mixing a pure tantalum powder having a particle size of 15 ⁇ with stearic acid at a volume ratio of 70:30, and then grinding it through a 200 mesh screen to agglomerate the powder into a powder. Larger particles, but no agglomeration between the particles and the particles; The good mixed sputum particles are transported onto the 3D printing platform, rolled and layered, and the sample size to be prepared is designed to be ⁇ 10 X 100 and the UG file is input into the 3D printing device. According to the information of each layer cross section of the sample, The print head has a jet mass concentration of 1 on the mixed tantalum powder particles. /.
• the ⁇ -cyanoacrylate adhesive forms a two-dimensional plane, and each layer of the adhesive is sprayed 3 times. After processing one layer, the workbench is lowered by 80 ⁇ m, and the next layer is processed, and layer-by-layer stacking is formed until After the final sample is completed, after the sample is molded, the mixed tantalum powder particles which are not stuck on the surface are removed and left for 24 hours; then the sample is subjected to degreasing, high-temperature sintering and cooling, etc., and the post-treatment steps are carried out at a rate of 3 ° C/min.
• a method for preparing a porous sputum medical implant material firstly having a purity of 20 ⁇ m
• the tantalum powder and zinc stearate are thoroughly mixed at a volume ratio of 60:40, and then ground through a 200 mesh screen to agglomerate the powder into larger particles, but the particles are not agglomerated with the particles;
• the particles are transported onto the three-dimensional printing platform, the laminate is rolled, the sample to be prepared is designed, and the UG file is input into the three-dimensional printing device.
• the print head is mixed with the powder particles.
• the ⁇ -cyanoacrylate adhesive with a spray concentration of 0.8% forms a two-dimensional plane, and each layer of the adhesive is sprayed 3 times.
• the table is lowered by ⁇ , and the next layer is processed. , layer-by-layer build-up, until the final sample is completed, after the sample is formed, remove the mixed tantalum powder particles that are not stuck on the surface, and leave it for 24 hours; then de-fat, high-temperature sintering and cooling, etc. 1.2 ° C / min rate from room temperature to 400 ° C, holding 60min, argon gas inlet rate 1.
• OL / min from 400 ° C to 600 ° C at a rate of 0.5 ° C / min, insulation 120 Min, the vacuum is maintained at 1 X 10 - 3 Pa;
• sintering Raise from room temperature to 1250 ° C at a rate of 12 ° C / min, keep warm for 30 min, vacuum degree is 1 ⁇ 10 - 4 Pa; increase to 1500 ° C at 20 ° C / min, keep warm for 30 min, vacuum 1 10 - 4 Pa ⁇ l 10 - 3 Pa; 2200 ° C at 20 ° C / min, 4 h, vacuum 1 ⁇ 10 - 4 Pa; Cooling: 1 10" 4 Pa vacuum - 1 10— 3 Pa; cooled to 1500 ° C at a rate of 10 ° C / min, kept for 30 min; cooled to 1200 ° C at a rate of 20 ° C / min, kept 1.
• Examples 3 to 8 The following steps and process parameters were carried out, and the rest were the same as in Example 1.
• the rate of 3 13 ° C / min was raised from room temperature to 1220 ° C, and the annealing step was not performed.
• the degree of vacuum is 10 _3 Pa;
• the degree of vacuum is 10—;
• the degree of vacuum is 1 O ⁇ Pa ⁇ 10" ? Pa; at 20 °C / min
• Rate is cooled to 1600 ° C, ⁇ L 60 min;
• °C/min is cooled to 400 °C, and the temperature is raised to 1800 °C at a rate of 12 °C/min.
• the vacuum is 103 ⁇ 4;
• Cooling with the furnace The rate of 10 ° C / min is raised from room temperature to 1800 ° C, the degree of vacuum is 10 - 4 Pa ⁇ 10 - 3 Pa, and the temperature is raised to 850 at 15 ° C / min.
• vacuum is 10"3 ⁇ 4; to /im
• the degree of vacuum is 10 Pa;
• the degree of vacuum is 10" 3 ⁇ 4 ⁇ 10-; at 17 °C/min
• the rate is cooled to 1500 ° C, 50 min;
• the rate of 20 ° C / min was raised from room temperature to 1600 ° C without an annealing step.
• the degree of vacuum is 10 - 3 Pa
• the degree of vacuum is l (TPa ⁇ 10— ; 14°C/min
• the rate is cooled to 1520 ° C, 55 min;
• the rate of 14 ° C / min rises from room temperature to 1230 ° C, the degree of vacuum is 10 - 4 Pa ⁇ 10 - 3 Pa, 50 minutes, the degree of vacuum is 10 to 13 ° C / min, the temperature is raised to 820 to 17 ° C / The rate of min is raised to 1500 ° C, the temperature is kept at ° C, the temperature is kept for 350 min, and then 3
• the degree of vacuum is l (TPa; °C / min cooled to 400 ° C, the temperature is raised to 2160 ° C at 11 ° C / min, held for 150 min, and then cooled with the furnace
• vacuum is 10"3 ⁇ 4; to jm
• the degree of vacuum is 10 & ⁇ 10 _ ; at 13 ° C / min Rate was cooled to 1600 ° C, 35 min;
• vacuum 10 is heated at 18 °C / min to 870 to 14 ° C / min to 1500 ° C, keep warm ° C, keep warm 420 min, then 4
• vacuum is 103 ⁇ 4; °C/min is cooled to 400°C, and the temperature is raised to 2150°C, 230min at 8°C/min, and then cooled to the furnace.
• the degree of vacuum is 10—; to yjoi.
• the degree of vacuum is 10" 3 ⁇ 4 ⁇ 10-3 Pa; at 17 °C/min
• the obtained porous tantalum product has three-dimensional complete connectivity, pore-to-hook distribution, and good biocompatibility.
• the test results are as follows:

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• Oral & Maxillofacial Surgery (AREA)
• Transplantation (AREA)
• Epidemiology (AREA)
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• Automation & Control Theory (AREA)
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• 2012
  • 2012-01-31 CN CN201210022122.1A patent/CN102796909B/zh active Active
  • 2012-12-31 WO PCT/CN2012/088143 patent/WO2013113248A1/fr not_active Ceased

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