CN108653820A - A kind of preparation method of porous metals bone inlay object - Google Patents
A kind of preparation method of porous metals bone inlay object Download PDFInfo
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- CN108653820A CN108653820A CN201810526901.2A CN201810526901A CN108653820A CN 108653820 A CN108653820 A CN 108653820A CN 201810526901 A CN201810526901 A CN 201810526901A CN 108653820 A CN108653820 A CN 108653820A
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- 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
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- 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
-
- 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
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
-
- 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
- A61L27/14—Macromolecular materials
- A61L27/16—Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- A61L27/14—Macromolecular materials
- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
-
- 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
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
-
- 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
-
- 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
Abstract
The invention discloses a kind of preparation methods of porous metals bone inlay object, belong to bone renovating material field, its purpose is to provide a kind of precision of manufacturing process higher, the preparation method of the better porous metals bone inlay object of the structural stability of resulting product.The present invention includes the following steps：It configures poly-vinyl alcohol solution, configuration metal powder/polyvinyl alcohol pulp, mold, fill mould, gel, dissolving, drying, sintering.The preparation method of the present invention is not limited to the type of metal material, and the pore size of obtained porous metals bone inlay object is easily controllable, and whole form is adjustable, and stable structure, reliable in mechanical performance are high, entire technological process is simple, and environmental requirement is low, manufacturing cost is low, and replicability is high.
Description
Technical field
The invention belongs to bone renovating material fields, and in particular to a kind of porous metals bone inlay object preparation method.
Background technology
The a variety of causes such as traffic accident, accident and disease can all cause a large amount of skeleton trauma and bone defect disease every year
Example, and clinically generally require and these defect wounds are filled with bone inlay object, to reach mechanical support and help bone
The purpose of organization healing.In practice process, the inner matter of porous metals (such as titanium, tantalum) manufacture is because it is with good mechanics
Performance and biological safety, therefore be widely used in bone defect healing.
The technology for having some more mature at present has applied to manufacture the porous inner matter of different metal material, such as logical
Chemical vapor deposition technology is crossed using chemical reaction in porous surface deposited metal；Although this method can obtain height
It is even, the porous tantalum of the complete unicom of hole；But the disadvantage is that this method is only used for several metallic elements such as tantalum, it is impossible to be used in manufacture
POROUS TITANIUM etc.；In addition, this method uses special equipment (gas-phase chemical reaction device), it is related to complicated condition control and operated
Journey, cost are very high.
In addition it can carry out the manufacture of porous inner matter by polymeric foam template, the advantages of this method is unlimited
In the type of metal material and without using special installation, but the disadvantage is that binder used in the fabrication process often has height
Viscosity and film forming, therefore usually a remaining tunic, this tunic ultimately become one layer at the outs open in hole in technical process
Metal causes part hole to become closed pore, it has been experienced that this defect is difficult to avoid；In addition, this technics comparing is simple, but
Dependent on manual skill, there is very big defect in the stability of technique.
Also particle packing template can also realize the manufacture of porous inner matter, although this method cost is relatively low, one
As can only manufacture the relatively simple porous metals of form, and the porous metals with particular design form can not be manufactured, therefore transport
It is relatively narrow with range.
It for another example says and 3D printing is carried out by electron beam or laser, although any form may be implemented in this method in principle
The printing manufactures of porous metals print material but since metal 3D printing equipment cost and its operation and maintenance are costly
Material it is also costly, and print metal inside be easy hole and thermal stress, cause the strength of materials relatively low, easy to produce fatigue and
Brittle failure even occurs for abrasion, thus there is limitation in popularization and application.Further, since 3D printing essence is melting, soon for metal
Fast cooling procedure, therefore be easy to form the metallographic structure of nonequilibrium state (supersaturation) during being quickly cooled down.Such as, the 3D of titanium is beaten
Print can form titanium martensite.And the free energy of the tissue of nonequilibrium state is higher than equilibrium state tissue, therefore corrosion rate is also above flat
Weigh state tissue.
Application No. is the patent of invention of CN201610439554.0 disclose it is a kind of be used for 3D printing artificial bone material, it is described
Material is grouped as by following group by weight：40~60 parts of biological metal powder, 30~40 parts of non-metal powder, makrolon
20~32 parts, 5~8 parts of povidone k30,0.5~0.7 part of niacin, 0.02~0.1 part of dopamine.The artifical bone that the invention provides
Not only intensity is high for material, but also passes through the effect of dopamine, niacin, povidone k30 and other materials in component so that boniness
Bone joint interface such as is decomposed, absorbs, being precipitated at the reactions, can realize strong bonded with bone, prevents fatigue and abrasion, and should
The material that invention provides overcome in the case where not aggravating unit material weight in current material in easy engagement activity and
Caused by the influence of internal acid medium the technical issues of the stress decrease of material, the stress of material is substantially increased.
But by analyze the patent it can be found that its biological metal powder the mass ratio upper limit be 60 parts, poly- carbonic acid
The lower limit of ester is 20 parts, therefore the mass ratio of biological metal powder and makrolon is up to 60：20；Biological metal powder therein
By taking titanium as an example, the density of titanium is 4.2g/cm at end3, and the density of makrolon is 0.92g/cm3To 1.2g/cm3Between, it takes here
Makrolon density is 1.2；Therefore can be up to (60/4.2) by the way that titanium and makrolon volume ratio is calculated:(20/
1.2)=14.29:16.67.It can be found that the volume accounting of biological metal powder is less than 50%.Therefore, by described in the patent
" dumping " processing after, polycarbonate portion can all become the hole between metal powder and periphery, and the totality of its hole
Total volume of the product more than metal powder.It is gained knowledge according to material and is known that the stability of this structure can be very fragile, be easy to collapse
It dissipates, therefore controllability is poor in actual mechanical process, there are disadvantages for robustness and replicability.
Invention content
It is an object of the invention to：A kind of preparation method of porous metals bone inlay object is provided, this kind of preparation method is unlimited
Easily controllable in the pore size of the type of metal material, obtained porous metals bone inlay object, whole form is adjustable, and
Stable structure, reliable in mechanical performance are high, and entire technological process is simple, and environmental requirement is low, and manufacturing cost is low, and replicability is high.
The technical solution adopted by the present invention is as follows：
A kind of preparation method of porous metals bone inlay object, which is characterized in that include the following steps：
(1) poly-vinyl alcohol solution is configured：The pva powder of 2.5~7 parts of weight is taken to be dissolved in the hot water of 100 parts of weight
In, poly-vinyl alcohol solution is formed after polyvinyl alcohol is completely dissolved, poly-vinyl alcohol solution is cooled to room temperature；
(2) metal powder/polyvinyl alcohol pulp is configured：The metal powder of 45~80 parts of weight is taken to be dispersed in step (1) system
In the poly-vinyl alcohol solution obtained, stirring forms metal powder/polyvinyl alcohol pulp；
(3) mold：Low melting material is printed with 3D printer becomes bone inlay object template；
(4) mould is filled：Metal powder made from step (2)/polyvinyl alcohol pulp is injected under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template made from step (3)；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；
(6) it dissolves：The gel obtained with solvent processing step (5) compatible with low melting material in step (3), dissolving
Low melting material template in gel, obtains dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is dried, removes moisture removal；
(8) it is sintered：By the dimensional perfusion body vacuum-sintering after step (7) is dry, porous metals bone inlay object is made.
Wherein, the polyvinyl alcohol average degree of polymerization in step (1) is not less than 1700, and hot water temperature is higher than 90 DEG C.
Wherein, metal powder is titanium, tantalum or Ti-6Al-4V in step (2).
Wherein, low melting material is paraffin, polylactic acid or nylon in step (3).
Wherein, increase step (5.1) between step (5) and step (6),
Step (5.1)：Gel after step (5) natural cooling is put into refrigerator after being chilled to 0 DEG C to -20 DEG C, followed by
Gel after freezing is taken out clear-cutting forestland to room temperature by continuous freezing 0.5 hour to 3 hours.
Wherein, step (5.1) is repeated at least twice.
Wherein, the solvent selected in step (6) is n-hexane compatible with paraffin used in step (3), Huo Zhewei
Dichloromethane compatible with polylactic acid, or be m-methyl phenol compatible with nylon.
Wherein, it is dried using baking oven in step (7), and the temperature of baking oven is 40 DEG C to 80 DEG C.
In conclusion by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
1, the present invention in, by using 3D printing bone inlay object template can by Mechanics Calculation then design most preferably by
The porous bone inlay object structure of power, while aperture, porosity can be also produced according to certain required rule variation with space
The porous bone inlay object structure of distribution of pores；In addition, using cheap low melting point for template in 3D printing, avoid directly
Using expensive metal 3D printer, technique manufacturing cost has been saved, meanwhile, the low melting materials such as paraffin, polylactic acid, nylon exist
The external environmental conditions such as high temperature, vacuum need not be provided when 3D printing, therefore it is a wide range of also further to improve the production technology
The advantage of popularization.On the other hand, a series of steps such as filling mould, gel, dissolving, drying, sintering are carried out by the template to 3D printing
Suddenly, obtained product not only has very high reliability in mechanical performance, but also can be found by experiment：Using this method
The aperture of manufacture is diameter >=200 μ of communicating passage between reaching at least 98% hole in 400 μm~700 μm of Porous titanium
m；And in contrast to the Porous titanium using the manufacture of particle packing template, in same apertures, there are about between 20% hole
There are local stenosis in channel, cause local diameter<200μm.Therefore the total quality of the obtained metal bone inlay object of the present invention
It is more excellent；Meanwhile the manufacturing process of whole process of the present invention is simple, production cost is low and is advantageous to industrial applications, is suitble to
Large-scale promotion.
2, in the present invention, setting polyvinyl alcohol average degree of polymerization is not less than 1700, this ensure that poly-vinyl alcohol solution is viscous
Degree is abundant, and metal and liquid phase in slurry is made not detach；In addition, molecular weight it is big polyvinyl alcohol cohesive force it is strong, impart so solidifying
It is defeated and dispersed to ensure that the bottling body after drying is not easy for glue and the sufficient intensity of dimensional perfusion body.Hot water temperature's setting is higher than 90 DEG C,
This ensure that polyvinyl alcohol is rapid, fully dissolves, guarantor is provided to prepare good metal powder/polyvinyl alcohol pulp
Barrier.
3, in the present invention, using titanium, tantalum or Ti-6Al-4V as the metal material for preparing porous metals bone inlay object, it
Have the characteristics such as higher-strength, corrosion-resistant, nontoxic to human body, therefore be more suitable for as original compared to general metal powder
Material prepares porous metals bone inlay object.
4, in the present invention, paraffin, polylactic acid or nylon is chosen and carries out 3D printing, ensure that printing template first in this way
Stability, in addition paraffin, polylactic acid and nylon convenient material drawing and price is more cheap, need not also provide in print procedure
The harsh environmental condition such as high temperature, vacuum, therefore easily manufactured and cost is relatively low, the more convenient present invention's promotes the use of.
5, in the present invention, by thawing after being freezed gel, enhance the physical crosslinking of polyvinyl alcohol so that gel is whole
The structural behaviour of body is more excellent；By thawing after carrying out multiple freezing to gel, the knot of gel entirety is further enhanced
The stability of structure performance, the dimensional perfusion body to being obtained after dissolving low melting material template is obviously improved.
6, in the present invention, a temperature appropriate, is conducive to removal three between oven temperature is set to 40 DEG C to 80 DEG C
Bottling body internal moisture is tieed up, follow-up vacuum-sintering is made to be carried out, the final stability for realizing porous metals bone inlay object entirety
And mechanical strength.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, by the following examples to the present invention
It is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit
The fixed present invention.
Embodiment 1
A kind of preparation method of porous metals bone inlay object, includes the following steps：
(1) poly-vinyl alcohol solution is configured：The pva powder that 2.5 parts of weight and average degree of polymerization are 1750 is taken to be dissolved in
The temperature of 100 parts of weight is to form poly-vinyl alcohol solution after polyvinyl alcohol is completely dissolved in 95 DEG C of hot water, and polyvinyl alcohol is molten
Liquid is cooled to room temperature；
(2) titanium/polyvinyl alcohol pulp is configured：The titanium valve of 50 parts of weight is taken to be dispersed in polyvinyl alcohol made from step (1) molten
In liquid, stirring forms titanium/polyvinyl alcohol pulp；
(3) mold：Appropriate paraffin is taken, paraffin printing is become into bone inlay object template using 3D printer；
(4) mould is filled：By titanium made from step (2)/polyvinyl alcohol pulp injection step (3) under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template obtained；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；By gel
It is put into refrigerator and is chilled to -5 DEG C, and kept for 3 hours, the template after freezing-slurry complex is taken out into clear-cutting forestland to room
Temperature repeats the step 6 time of follow-up freeze-thaw.
(6) it dissolves：The gel for taking appropriate n-hexane processing step (5) to obtain, the paraffin in n-hexane dissolution gel, obtains
Dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is placed in the baking oven that temperature is 60 DEG C and is dried, removes
Moisture in dimensional perfusion body；
(8) it is sintered：Dimensional perfusion body after step (7) is dry is sintered, porous metals bone inlay object is made.
Embodiment 2
Porous metals bone inlay object is prepared, is included the following steps：
(1) poly-vinyl alcohol solution is configured：The pva powder that 5 parts of weight and average degree of polymerization are 2400 is taken to be dissolved in
The temperature of 100 parts of weight is to form poly-vinyl alcohol solution after polyvinyl alcohol is completely dissolved in 95 DEG C of hot water, and polyvinyl alcohol is molten
Liquid is cooled to room temperature；
(2) titanium/polyvinyl alcohol pulp is configured：The titanium valve of 80 parts of weight is taken to be dispersed in polyvinyl alcohol made from step (1) molten
In liquid, stirring forms titanium/polyvinyl alcohol pulp；
(3) mold：Appropriate paraffin is taken, paraffin printing is become into bone inlay object template using 3D printer；
(4) mould is filled：By titanium made from step (2)/polyvinyl alcohol pulp injection step (3) under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template obtained；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；By gel
It is put into refrigerator and is chilled to -20 DEG C, and kept for 1 hour, the template after freezing-slurry complex is taken out into clear-cutting forestland to room
Temperature repeats the step 4 time of follow-up freeze-thaw.
(6) it dissolves：The gel for taking appropriate n-hexane processing step (5) to obtain, the paraffin in n-hexane dissolution gel, obtains
Dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is placed in the baking oven that temperature is 55 DEG C and is dried, removes
Moisture in dimensional perfusion body；
(8) it is sintered：By the dimensional perfusion body vacuum-sintering after step (7) is dry, porous metals bone inlay object is made.
Embodiment 3
Porous metals bone inlay object is prepared, is included the following steps：
(1) poly-vinyl alcohol solution is configured：The pva powder that 7 parts of weight and average degree of polymerization are 1750 is taken to be dissolved in
The temperature of 100 parts of weight is to form poly-vinyl alcohol solution after polyvinyl alcohol is completely dissolved in 95 DEG C of hot water, and polyvinyl alcohol is molten
Liquid is cooled to room temperature；
(2) titanium/polyvinyl alcohol pulp is configured：The titanium valve of 80 parts of weight is taken to be dispersed in polyvinyl alcohol made from step (1) molten
In liquid, stirring forms titanium/polyvinyl alcohol pulp；
(3) mold：Appropriate polylactic acid is taken, polylactic acid printing is become into bone inlay object template using 3D printer；
(4) mould is filled：By titanium made from step (2)/polyvinyl alcohol pulp injection step (3) under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template obtained；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；By gel
It is put into refrigerator and is chilled to -20 DEG C, and kept for 2 hours, the template after freezing-slurry complex is taken out into clear-cutting forestland to room
Temperature repeats the step 4 time of follow-up freeze-thaw.
(6) it dissolves：The gel for taking q. s. methylene chloride processing step (5) to obtain, dichloromethane dissolve the poly- breast in gel
Acid obtains dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is placed in the baking oven that temperature is 55 DEG C and is dried, removes
Moisture in dimensional perfusion body；
(8) it is sintered：By the dimensional perfusion body vacuum-sintering after step (7) is dry, porous metals bone inlay object is made.
Embodiment 4
Porous metals bone inlay object is prepared, is included the following steps：
(1) poly-vinyl alcohol solution is configured：The pva powder that 3 parts of weight and average degree of polymerization are 1750 is taken to be dissolved in
The temperature of 100 parts of weight is to form poly-vinyl alcohol solution after polyvinyl alcohol is completely dissolved in 95 DEG C of hot water, and polyvinyl alcohol is molten
Liquid is cooled to room temperature；
(2) tantalum/polyvinyl alcohol pulp is configured：The tantalum powder of 50 parts of weight is taken to be dispersed in polyvinyl alcohol made from step (1) molten
In liquid, stirring forms tantalum/polyvinyl alcohol pulp；
(3) mold：Appropriate paraffin is taken, paraffin printing is become into bone inlay object template using 3D printer；
(4) mould is filled：By tantalum made from step (2)/polyvinyl alcohol pulp injection step (3) under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template obtained；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；By gel
It is put into refrigerator and is chilled to -5 DEG C, and kept for 2.5 hours, the template after freezing-slurry complex is taken out into clear-cutting forestland to room
Temperature repeats the step 5 time of follow-up freeze-thaw.
(6) it dissolves：The gel for taking appropriate n-hexane processing step (5) to obtain, the paraffin in n-hexane dissolution gel, obtains
Dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is placed in the baking oven that temperature is 55 DEG C and is dried, removes
Moisture in dimensional perfusion body；
(8) it is sintered：By the dimensional perfusion body vacuum-sintering after step (7) is dry, porous metals bone inlay object is made.
Embodiment 5
Porous metals bone inlay object is prepared, is included the following steps：
(1) poly-vinyl alcohol solution is configured：The pva powder that 6 parts of weight and average degree of polymerization are 2400 is taken to be dissolved in
The temperature of 100 parts of weight is to form poly-vinyl alcohol solution after polyvinyl alcohol is completely dissolved in 95 DEG C of hot water, and polyvinyl alcohol is molten
Liquid is cooled to room temperature；
(2) tantalum/polyvinyl alcohol pulp is configured：The tantalum powder of 70 parts of weight is taken to be dispersed in polyvinyl alcohol made from step (1) molten
In liquid, stirring forms tantalum/polyvinyl alcohol pulp；
(3) mold：Appropriate polylactic acid is taken, polylactic acid printing is become into bone inlay object template using 3D printer；
(4) mould is filled：By tantalum made from step (2)/polyvinyl alcohol pulp injection step (3) under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template obtained；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；By gel
It is put into refrigerator and is chilled to -5 DEG C, and kept for 2.5 hours, the template after freezing-slurry complex is taken out into clear-cutting forestland to room
Temperature repeats the step 5 time of follow-up freeze-thaw.
(6) it dissolves：The gel for taking q. s. methylene chloride processing step (5) to obtain, dichloromethane dissolve the poly- breast in gel
Acid obtains dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is placed in the baking oven that temperature is 55 DEG C and is dried, removes
Moisture in dimensional perfusion body；
(8) it is sintered：By the dimensional perfusion body vacuum-sintering after step (7) is dry, porous metals bone inlay object is made.
Embodiment 6
Porous metals bone inlay object is prepared, is included the following steps：
(1) poly-vinyl alcohol solution is configured：The pva powder that 6 parts of weight and average degree of polymerization are 2400 is taken to be dissolved in
The temperature of 100 parts of weight is to form poly-vinyl alcohol solution after polyvinyl alcohol is completely dissolved in 95 DEG C of hot water, and polyvinyl alcohol is molten
Liquid is cooled to room temperature；
(2) tantalum/polyvinyl alcohol pulp is configured：The tantalum powder of 70 parts of weight is taken to be dispersed in polyvinyl alcohol made from step (1) molten
In liquid, stirring forms tantalum/polyvinyl alcohol pulp；
(3) mold：Appropriate nylon is taken, nylon printing is become into bone inlay object template using 3D printer；
(4) mould is filled：By tantalum made from step (2)/polyvinyl alcohol pulp injection step (3) under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template obtained；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；By gel
It is put into refrigerator and is chilled to -5 DEG C, and kept for 2.5 hours, the template after freezing-slurry complex is taken out into clear-cutting forestland to room
Temperature repeats the step 5 time of follow-up freeze-thaw.
(6) it dissolves：The gel for taking appropriate methylphenol processing step (5) to obtain, methylphenol dissolve the nylon in gel,
Obtain dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is placed in the baking oven that temperature is 55 DEG C and is dried, removes
Moisture in dimensional perfusion body；
(8) it is sintered：By the dimensional perfusion body vacuum-sintering after step (7) is dry, porous metals bone inlay object is made.
Embodiment 7
Porous metals bone inlay object is prepared, is included the following steps：
Poly-vinyl alcohol solution is configured in (1)：The pva powder that 2.5 parts of weight and average degree of polymerization are 1750 is taken to dissolve
It is poly-vinyl alcohol solution to be formed after polyvinyl alcohol is completely dissolved, by polyvinyl alcohol in 93 DEG C of hot water in the temperature of 100 parts of weight
Solution is cooled to room temperature；
(2) Ti-6Al-4V/ polyvinyl alcohol pulps are configured：It takes the Ti-6Al-4V of 50 parts of weight to be dispersed in step (1) to be made
Poly-vinyl alcohol solution in, stirring form Ti-6Al-4V/ polyvinyl alcohol pulps；
(3) mold：Appropriate paraffin is taken, paraffin printing is become into bone inlay object template using 3D printer；
(4) mould is filled：Ti-6Al-4V/ polyvinyl alcohol pulps made from step (2) are injected under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template made from step (3)；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；By gel
It is put into refrigerator and is chilled to -20 DEG C, and kept for 0.5 hour, the template after freezing-slurry complex is taken out into clear-cutting forestland and is arrived
Room temperature repeats the step 8 time of follow-up freeze-thaw.
(6) it dissolves：The gel for taking appropriate n-hexane processing step (5) to obtain, the paraffin in n-hexane dissolution gel, obtains
Dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is placed in the baking oven that temperature is 60 DEG C and is dried, removes
Moisture in dimensional perfusion body；
(8) it is sintered：By the dimensional perfusion body vacuum-sintering after step (7) is dry, porous metals bone inlay object is made.
Embodiment 8
Porous metals bone inlay object is prepared, is included the following steps：
(1) poly-vinyl alcohol solution is configured：The pva powder that 4 parts of weight and average degree of polymerization are 2400 is taken to be dissolved in
The temperature of 100 parts of weight is to form poly-vinyl alcohol solution after polyvinyl alcohol is completely dissolved in 95 DEG C of hot water, and polyvinyl alcohol is molten
Liquid is cooled to room temperature；
(2) Ti-6Al-4V/ polyvinyl alcohol pulps are configured：It takes the Ti-6Al-4V of 60 parts of weight to be dispersed in step (1) to be made
Poly-vinyl alcohol solution in, stirring form Ti-6Al-4V/ polyvinyl alcohol pulps；
(3) mold：Appropriate polylactic acid is taken, polylactic acid printing is become into bone inlay object template using 3D printer；
(4) mould is filled：Ti-6Al-4V/ polyvinyl alcohol pulps made from step (2) are injected under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template made from step (3)；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；By gel
It is put into refrigerator and is chilled to -10 DEG C, and kept for 1.5 hours, the template after freezing-slurry complex is taken out into clear-cutting forestland and is arrived
Room temperature repeats the step 6 time of follow-up freeze-thaw.
(6) it dissolves：The gel for taking q. s. methylene chloride processing step (5) to obtain, dichloromethane dissolve the poly- breast in gel
Acid obtains dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is placed in the baking oven that temperature is 60 DEG C and is dried, removes
Moisture in dimensional perfusion body；
(8) it is sintered：By the dimensional perfusion body vacuum-sintering after step (7) is dry, porous metals bone inlay object is made.
Embodiment 9
Porous metals bone inlay object is prepared, is included the following steps：
(1) poly-vinyl alcohol solution is configured：The pva powder that 7 parts of weight and average degree of polymerization are 2400 is taken to be dissolved in
The temperature of 100 parts of weight is to form poly-vinyl alcohol solution after polyvinyl alcohol is completely dissolved in 95 DEG C of hot water, and polyvinyl alcohol is molten
Liquid is cooled to room temperature；
(2) Ti-6Al-4V/ polyvinyl alcohol pulps are configured：It takes the Ti-6Al-4V of 80 parts of weight to be dispersed in step (1) to be made
Poly-vinyl alcohol solution in, stirring form Ti-6Al-4V/ polyvinyl alcohol pulps；
(3) mold：Appropriate nylon is taken, nylon printing is become into bone inlay object template using 3D printer；
(4) mould is filled：Ti-6Al-4V/ polyvinyl alcohol pulps made from step (2) are injected under normal pressure or pressurized conditions
Template-slurry complex is formed in bone inlay object template made from step (3)；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；By gel
It is put into refrigerator and is chilled to -10 DEG C, and kept for 3 hours, the template after freezing-slurry complex is taken out into clear-cutting forestland to room
Temperature repeats the step 6 time of follow-up freeze-thaw.
(6) it dissolves：The gel for taking appropriate methylphenol processing step (5) to obtain, methylphenol dissolve the nylon in gel,
Obtain dimensional perfusion body；
(7) dry：The dimensional perfusion body that step (6) obtains is placed in the baking oven that temperature is 60 DEG C and is dried, removes
Moisture in dimensional perfusion body；
(8) it is sintered：By the dimensional perfusion body vacuum-sintering after step (7) is dry, porous metals bone inlay object is made.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (8)
1. a kind of preparation method of porous metals bone inlay object, which is characterized in that include the following steps：
(1) poly-vinyl alcohol solution is configured：It takes the pva powder of 2.5~7 parts of weight to be dissolved in the hot water of 100 parts of weight, waits for
Polyvinyl alcohol forms poly-vinyl alcohol solution after being completely dissolved, and poly-vinyl alcohol solution is cooled to room temperature；
(2) metal powder/polyvinyl alcohol pulp is configured：The metal powder of 45~80 parts of weight is taken to be dispersed in step (1) obtained
In poly-vinyl alcohol solution, stirring forms metal powder/polyvinyl alcohol pulp；
(3) mold：Low melting material is printed with 3D printer becomes bone inlay object template；
(4) mould is filled：By metal powder/polyvinyl alcohol pulp injection step made from step (2) under normal pressure or pressurized conditions
(3) template-slurry complex is formed in bone inlay object template made from；
(5) gel：Template made from step (4)-slurry complex cooled to room temperature is formed into gel；
(6) it dissolves：The gel obtained with solvent processing step (5) compatible with low melting material in step (3) dissolves gel
Interior bone inlay object template, obtains dimensional perfusion body；
(7) dry：Dimensional perfusion soma that step (6) obtains is dry, remove moisture removal；
(8) it is sintered：Dimensional perfusion body after step (7) is dry is sintered, porous metals bone inlay object is made.
2. a kind of preparation method of porous metals bone inlay object as described in claim 1, which is characterized in that in step (1)
Polyvinyl alcohol average degree of polymerization is not less than 1700, and hot water temperature is higher than 90 DEG C.
3. a kind of preparation method of porous metals bone inlay object as described in claim 1, which is characterized in that golden in step (2)
Category powder is titanium, tantalum or Ti-6Al-4V.
4. a kind of preparation method of porous metals bone inlay object as described in claim 1, which is characterized in that low in step (3)
Melting material is paraffin, polylactic acid or nylon.
5. a kind of preparation method of porous metals bone inlay object as described in claim 1, which is characterized in that step (5) with
Increase step (5.1) between step (6),
Step (5.1)：Gel after step (5) natural cooling is put into refrigerator after being chilled to 0 DEG C to -20 DEG C, is further continued for cold
Freeze 0.5 hour to 3 hours, the gel after freezing is taken out into clear-cutting forestland to room temperature.
6. a kind of preparation method of porous metals bone inlay object as claimed in claim 5, which is characterized in that repeat step
(5.1) at least twice.
7. a kind of preparation method of porous metals bone inlay object as claimed in claim 4, which is characterized in that choosing in step (6)
Solvent be n-hexane compatible with paraffin, be either dichloromethane compatible with polylactic acid or be and nylon phase
The m-methyl phenol of adaptation.
8. a kind of preparation method of porous metals bone inlay object as described in claim 1, which is characterized in that step is adopted in (7)
It is dried with baking oven, and the temperature of baking oven is 40 DEG C to 80 DEG C.
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