CN103740964A - Preparation method of medical porous metal implant material - Google Patents
Preparation method of medical porous metal implant material Download PDFInfo
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Abstract
The invention relates to a preparation method of a medical porous metal implant material. The method comprises the following steps: mixing tantalum powder with a pore former and a forming agent so as to form mixed powder; and performing granulation, injection mould forming, demoulding, degreasing, sintering and heat treatment on the mixed powder so as to prepare the medical porous metal implant material capable of replacing a dentale tissue, wherein the pore former is one or more of sodium bicarbonate, urea, sodium chloride, methylcellulose and ethyecellulose; the forming agent is one or more of polyvinyl alcohol, stearic acid, zinc stearate, paraffin and synthetic rubber; the degreasing process is performed under the conditions of gradually heating to 400 DEG C to 800 DEG C according to the speed rate of 0.5 DEG C/minute to 3 DEG C/minute, forming a protective atmosphere in an argon leading-in mode and carrying out heat preservation for 60 to 240 minutes; the sintering process and the heat treatment process are effectively improved. Thus, the mechanical property of the prepared medical porous metal implant material is greatly improved. As a result, the prepared medical porous metal implant material is very suitable for replacement of the dentale tissue.
Description
The present patent application is application number 201110296596.0, the applying date on 09 29th, 2011, and denomination of invention " a kind of preparation method of medical porous metal implant material " divides an application.
Technical field
The present invention relates to a kind of preparation method of medical metal implanted material, especially relate to a kind of preparation method of medical porous metal implant material.
Background technology
Porous medical metal implanted material has treatment osseous tissue wound, bone formation necrosis and alternative dense bone tissue as important and special purposes such as dentales, and existing this common class material has porous metal stainless steel, porous metal titanium etc.Porous embedded material as osseous tissue wound and the use of bone formation necrosis therapeutic, its porosity should reach 30～80%, and hole is preferably all communicated with and is uniformly distributed, or make it as required both consistent with the bone growth of human body, alleviate again the weight of material itself, to be applicable to human body, implanted use.
And refractory metals tantalum, because it has outstanding biocompatibility, its porous material is expected to the conventional medical metallic biomaterial such as aforementioned as an alternative.Due to metal tantalum to human body harmless, nontoxic, have no side effect, and along with the develop rapidly of domestic and international medical science, tantalum is goed deep into as the further of body implanting material cognition, and people implant and become more and more urgent by the demand of porous metal tantalum material human body, also more and more higher to its requirement.Wherein, as the medical embedded metal tantalum of porous, if can have the very high physical and mechanical properties that is uniformly distributed open pore and adapts with human body, it is expected to as a kind of novel osseous tissue equivalent material.
As medical embedded porous metal material, just as one porous metal material, be to take powder sintering as main working method substantially, in particular for obtain porosity communication and equally distributed porous metal foam structure adopt metal-powder slurry in the powder sintering dipping on Organic Foam Material afterwards the dry knot that reburns to be called for short foam impregnation method in the majority.About powder sintered obtained porous metal material conventionally its Metal Mechanic Property be not fine, its major cause is the problem of subsiding how arranging in technique in the support of pore-forming medium and elimination relation, metal powder sintered process.And in known bibliographical information, all there is no good solution and laissez-faire nature.
Adopt bibliographical information that metal powder sintered legal system makes porous tantalum seldom, particularly take and obtain medical embedded material and almost do not have with the porous tantalum powder sintering bibliographical information that is object.Can reference be that publication number is CN200510032174, title " three-dimensional through hole or part hole porous metal foam connected with each other and preparation method thereof " and CN200710152394, title " a kind of porous foam tungsten and preparation method thereof ".Yet porous metal that it obtains or for filtering material use, or share for aerospace and other high-temperature field but not use as medical metal implanted material, moreover also non-porous tantalum of the porous metal of processing.
About porous tantalum, US5282861 discloses a kind of perforate tantalum material and preparation thereof that is applied to spongy bone implant, cell and organizes susceptor.This porous tantalum is made by pure business tantalum, it take polyurethane precursor, and to carry out the carbon skeleton that thermal destruction obtains be support, this carbon skeleton is multiple dodecahedron, it in it, is mesh-like structure, integral body spreads all over micropore, porosity can be up to 98%, then the method by chemical vapour deposition, infiltration is attached on carbon skeleton to form porous metal microstructure, referred to as chemical deposition by commercially pure tantalum.Its surperficial tantalum layer thickness of the porous tantalum material that this method obtains is between 40～60 μ m; In whole porous material, tantalum heavily accounts for 99%, and carbon skeleton weight accounts for 1% left and right.Document is further recorded, the ultimate compression strength 50～70MPa of this porous material, Young's modulus 2.5～3.5GPa, tensile strength 63MPa, amount of plastic deformation 15%.But using it as dense bone tissue as the porous tantalum of the medical embedded materials such as dentale, the mechanical property of its material has obvious weak point as ductility, ultimate compression strength, flexural strength etc., and can have influence on the follow-up processing to porous tantalum material itself, such as cutting of profiled member etc.Also all there is such deficiency in the same product obtaining in aforesaid metal powder sintered method.
Summary of the invention
The object of the present invention is to provide the preparation method of the medical porous metal implant material that a kind of biocompatibility and mechanical property are good.
The object of the invention is to realize by following technique means:
A kind of preparation method of medical porous metal implant material, tantalum powder and pore-forming material, forming agent are mixed into mixed powder, then through granulation, be injected into mould molding, the demoulding, degreasing, sintering and thermal treatment and make the medical porous metal implant material that substitutes dentale tissue; It is characterized in that: described pore-forming material is one or more in sodium bicarbonate, urea, sodium-chlor, methylcellulose gum, ethyl cellulose, described forming agent is one or more in polyvinyl alcohol, stearic acid, Zinic stearas, paraffin, synthetic rubber; Described skimming processes is that the speed with 0.5 ℃/min～3 ℃/min is progressively warming up to 400～800 ℃, with argon gas, passes into and forms protective atmosphere and be incubated 60min～240min, and described sintering step is that vacuum tightness is 10
-4pa～10
-3pa, with 10～20 ℃/min, be warming up to 1500～1800 ℃, be incubated 120～240min, with stove, be chilled to 200～300 ℃, with 10～20 ℃/min, be warming up to 1500～1800 ℃, insulation 180～240min again, with 5～10 ℃/min, be warming up to 2000～2200 ℃, insulation 120～360min; Described heat treatment step is that vacuum tightness is 10
-4pa～10
-3pa, is warming up to 800～900 ℃, insulation 240～480min with 10～20 ℃/min, then is chilled to 400 ℃, insulation 120～300min with 2～5 ℃/min, then cools to room temperature with the furnace.
In the R&D process of medical porous tantalum material, syntheti c route is numerous, but contriver has creatively proposed to adopt above-mentioned processing step to prepare fine and close medical porous tantalum embedded material, the above-mentioned thermal treatment process particularly adopting, has eliminated fully internal stress, has made the toughness of organizing more evenly, greatly improved prepared porous tantalum material of porous tantalum material; Above-mentioned sintering processes technique, makes idiosome become heating element, more even, thorough thereby sintering obtains.
For the porous tantalum material porosity of the alternative dentale tissue that makes to make suitable so that biocompatibility excellent, improve the mechanical property of its material simultaneously, above-mentioned granulation process is to be that 450～650 ℃, operating pressure are under 12～15MPa, described mixed powder to be a granulated into particle diameter not higher than the circular granular of 20 μ m in working temperature, and the temperature that described circular granular is injected into mould is that 380～540 ℃, pressure are 72～90MPa.
The median size of the Ta powder that the present invention adopts is less than 43 microns, oxygen level is less than 0.1%, is commercially available prod; Above-mentioned pore-forming material, forming agent are also commercially available prod.It is 10 that vacuum environment of the present invention preferably adopts vacuum tightness
-4pa～10
-3the vacuum condition of Pa.
In R&D process, contriver further studies discovery, if control bad in above-mentioned preparation, though can make and be suitable for as mentioned above substituting the medical embedded material of dentale but conforming product rate is not high: as difficult in powder pressing forming, be prone to layering, inhomogeneous in compacting rear section, degreasing rear section there will be the technical problems such as crackle.
In order to make in powder compaction process moulding easier, thereby raising yield rate, finished product hole homogeneity, make preparation process more stable, in above-mentioned mixed powder, the consumption of forming agent is 5～10%, the consumption of pore-forming material is 20～30%, surplus is tantalum powder, in volumn concentration, (in volumn concentration, be the unit of directly calculating by the situation of final porous tantalum material, in above-mentioned mixed powder weighs or according to the densometer of respective substance, calculate its corresponding quality weighing), more preferably forming agent is that paraffin accounts for 7～9%, pore-forming material is that ethyl cellulose accounts for 26～29%, surplus is tantalum powder, further be preferably paraffin and account for 8%, ethyl cellulose accounts for 27%, surplus is tantalum powder, all in volumn concentration, above-mentioned demould time is preferably 6～9S, more preferably 7S.
In order to make in skimming processes idiosome more stable, reduce the part idiosome distortion being prone to, aperture is inhomogeneous, thereby further improve yield rate, quality of production stability, in the preparation of the porous tantalum material of above-mentioned alternative dentale tissue, skimming processes is preferably progressively warming up to 400～800 ℃ with the speed of 2.5～3 ℃/min, with argon gas, pass into and form protective atmosphere and be incubated 150min～240min, further preferably with the speed of 2.5 ℃/min, be progressively warming up to 400～800 ℃, with argon gas, pass into and form protective atmosphere and be incubated 220min, most preferably, above-mentioned degreasing is that the speed with 1～3 ℃/min rises to 400 ℃ from room temperature, insulation 60～120min, speed with 1.5～2.5 ℃/min rises to 600～800 ℃ from 400 ℃, insulation 180～240min, the preferred temperature of above-mentioned granulation process is that 510～535 ℃, operating pressure are the circular granular that under 13MPa, described mixed powder is a granulated into particle diameter 10～20 μ m (more preferably 13 μ m), by the injection molding temperature of described circular granular, is that 465～490 ℃, pressure are 83～85MPa.
For make idiosome sintering obtain more evenly, thorough, make the medical porous tantalum strength of materials that makes higher, it is 10 that above-mentioned sintering step is preferably vacuum tightness
-4pa～10
-3pa, with 12～15 ℃/min, be warming up to 1500～1800 ℃, be incubated 180～200min, with stove, be chilled to 200～300 ℃, with 16～19 ℃/min, be warming up to 1500～1800 ℃, insulation 220～240min again, with 5～10 ℃/min, be warming up to 2000～2200 ℃, insulation 250～320min; Further being preferably vacuum tightness is 10
-4pa～10
-3pa, is warming up to 1800 ℃, is incubated 200min, with stove, is chilled to 200～300 ℃ with 13 ℃/min, then is warming up to 1800 ℃, insulation 230min with 17 ℃/min, with 7 ℃/min, is warming up to 2000～2200 ℃, insulation 300min.
Better in order to eliminate more fully internal stress, the toughness of material, above-mentioned heat treatment step is that vacuum tightness is 10
-4pa～10
-3pa, is warming up to 800～900 ℃, insulation 260～320min with 15 ℃/min, then is chilled to 400 ℃, insulation 120min with 3 ℃/min, then is cooled to room temperature with 18 ℃/min～23 ℃/min.
Cooling conditions after above-mentioned vacuum sintering also includes: vacuum tightness is not less than 10
-3pa, with not higher than 25 ℃/min, is not less than 10 ℃/min and gradually falls rate of cooling mode, and to sintered porous bodies segmentation cooling down to 800 ℃, each section of soaking time 30min～90min, then cools to normal temperature with the furnace.
Preferably, the cooling conditions after above-mentioned vacuum sintering is: vacuum tightness is 10
-4pa～10
-3pa; Speed with 10～20 ℃/min is cooled to 1500～1600 ℃, insulation 30～60min; Speed with 12～20 ℃/min is cooled to 1200～1250 ℃, insulation 60～90min; Speed with 10～20 ℃/min is cooled to 800 ℃, then furnace cooling.
The character of metal tantalum and niobium is extremely similar, and aforesaid method is equally also applicable to the preparation of medical porous niobium material.
Preparation methods for porous metal materials of the present invention has adopted injection moulding, makes the content of impurity in final porous tantalum material extremely low, has effectively improved biocompatibility and biological safety; Optimization of process conditions to granulation of the present invention, injection molding, degreasing, sintering and annealing steps, make that yield rate is high, finished product aperture homogeneity is better, make that preparation process is more stable, quality stability good, effectively eliminated thermal stresses, made organizing of porous tantalum material more even, with the mechanical property that further improves porous tantalum, be all improved as intensity, toughness simultaneously.The above-mentioned thermal treatment process particularly adopting, has eliminated fully internal stress, has made the toughness of organizing more evenly, greatly improved prepared porous tantalum material of porous tantalum material; Above-mentioned sintering processes technique, makes idiosome become heating element, more even, thorough thereby sintering obtains.As everyone knows, the qualification rate of product, production stability are determined by manual operation factor and operational path itself determines, manual operation can be tending towards normal level in high standardization after all, therefore quality of production stability is mainly determined by technique own, its product qualified rate of preparation technology of the present invention is high, production is stable, and conforming product rate is up to 93.0%～95.0%.Porous tantalum finished product even pore distribution and connection that the present invention makes, good biocompatibility.For the porous tantalum material of the alternative dentale tissue making, through its foreign matter content of test can be lower than 0.2%, density reachable 11.67～13.34g/cm
3, porosity can reach 20～30%, and pore diameter can reach 12～25 μ m, Young's modulus can reach that 6.0～7.0Gpa, unit elongation reach 14.0～15.0%, flexural strength can reach 160～180Mpa, ultimate compression strength can reach 115～130Mpa.
Embodiment
Below by embodiment, the present invention is specifically described; be necessary to be pointed out that at this following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, person skilled in art can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
Embodiment 1: take paraffin, median size and be less than 43 microns of oxygen levels and be less than 0.1% tantalum powder and ethyl cellulose and be mixed into mixed powder, wherein paraffin accounts for 8%, ethyl cellulose accounts for 27%, tantalum powder accounts for 65%, all in volumn concentration.Granulation: be that 510～520 ℃, operating pressure are under 12～13MPa, described mixed powder to be a granulated into the circular granular of particle diameter 10～13 μ m in working temperature.Injection molding: the temperature that described circular granular is injected into mould is that 465～490 ℃, pressure are 83～85MPa.Demould time: 6～7S.Skimming treatment: vacuum tightness 10
-4pa, rises to 400 ℃ with the speed of 1～3 ℃/min from room temperature, and insulation 60～120min rises to 600～800 ℃, insulation 180～240min with the speed of 1.5～2.5 ℃/min from 400 ℃.Vacuum sintering: vacuum tightness is 10
-4pa～10
-3pa; with 13 ℃/min, be warming up to 1800 ℃, be incubated 200min, with stove, be chilled to 200～300 ℃, then be warming up to 1800 ℃, insulation 230min with 17 ℃/min, with 7 ℃/min, be warming up to 2000～2200 ℃, insulation 300min; the protection of sintering process applying argon gas, thermal treatment: vacuum tightness is 10
-4pa～10
-3pa, with 15 ℃/min, be warming up to 800～900 ℃, insulation 260～320min, then be chilled to 400 ℃, insulation 120min with 3 ℃/min, then be cooled to room temperature with 18 ℃/min～23 ℃/min, after taking out product, remove surface dirt and dirt, make porous tantalum finished product.
Contriver detects the porous material density of above-mentioned porous tantalum finished product, porosity, aperture and various mechanical property by standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001: its foreign matter content is lower than 0.2%, its even pore distribution, density 12.54g/cm
3, porosity 25%, hole mean diameter 23 μ m, Young's modulus 6.7GPa, unit elongation 14.8%, flexural strength 172MPa, ultimate compression strength 125MPa.This porous tantalum is suitable for substituting the medical embedded material of human body dentale tissue very much.
Embodiment 2: weighing polyvinyl alcohol, median size are less than 43 microns of oxygen levels and are less than 0.1% tantalum powder and sodium bicarbonate and are mixed into mixed powder, and wherein polyvinyl alcohol accounts for 6%, sodium bicarbonate accounts for 29%, tantalum powder accounts for 65%, all in volumn concentration.Granulation: be that 450 ℃, operating pressure are under 15MPa, described mixed powder to be a granulated into the circular granular of particle diameter 20 μ m in working temperature.Injection molding: the temperature that described circular granular is injected into mould is that 540 ℃, pressure are 90MPa.Demould time: 9S.Skimming treatment: vacuum tightness 10
-4pa, is warming up to 400 ℃, insulation 60min with the temperature rise rate of 1 ℃/min from room temperature; Temperature rise rate with 2.5 ℃/min is warming up to 800 ℃, soaking time 180 minutes from 400 ℃ again.Vacuum sintering: sintering step: vacuum tightness is 10
-4pa, is warming up to 1800 ℃, is incubated 240min, with stove, is chilled to 200～300 ℃ with 20 ℃/min, then is warming up to 1500 ℃, insulation 180min with 10 ℃/min, with 10 ℃/min, is warming up to 2000～2200 ℃, insulation 360min; After taking out product, remove surface dirt and dirt, heat treatment step: vacuum tightness is 10
-3pa, is warming up to 800～900 ℃, insulation 480min with 10 ℃/min, then is chilled to 400 ℃, insulation 300min with 2 ℃/min, then cools to room temperature with the furnace.The sample making carries out conventional aftertreatment again and obtains porous tantalum finished product.
Contriver detects the porous material density of above-mentioned porous tantalum finished product, porosity, aperture and various mechanical property by standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001: its foreign matter content is lower than 0.2%, its even pore distribution, density 11.74g/cm
3, porosity 30%, hole mean diameter 24 μ m, Young's modulus 6.1GPa, unit elongation 14.2%, flexural strength 163MPa, ultimate compression strength 117MPa.This porous tantalum is suitable for substituting the medical embedded material of human body dentale tissue very much.
Embodiment 3: take Zinic stearas, median size and be less than 43 microns of oxygen levels and be less than 0.1% tantalum powder and methylcellulose gum and be mixed into mixed powder, wherein Zinic stearas accounts for 10%, methylcellulose gum accounts for 23%, tantalum powder accounts for 67%, all in volumn concentration.Granulation: be that 650 ℃, operating pressure are under 12MPa, described mixed powder to be a granulated into the circular granular of particle diameter 10 μ m in working temperature.Injection molding: the temperature that described circular granular is injected into mould is that 380 ℃, pressure are 72MPa.Demould time: 6S.Skimming treatment: vacuum tightness 10
-4pa, is warming up to 400 ℃, insulation 120min with the temperature rise rate of 3 ℃/min from room temperature; Temperature rise rate with 1.5 ℃/min is warming up to 750 ℃, soaking time 240 minutes from 400 ℃ again; Sintering: vacuum tightness is 10
-3pa, is warming up to 1500 ℃, is incubated 120min, with stove, is chilled to 200～300 ℃ with 10 ℃/min, then is warming up to 1800 ℃, insulation 240min with 20 ℃/min, with 5 ℃/min, is warming up to 2000～2200 ℃, insulation 120min; Heat treatment step: vacuum tightness is 10
-4pa, is warming up to 800～900 ℃, insulation 240min with 20 ℃/min, then is chilled to 400 ℃, insulation 120min with 5 ℃/min, then cools to room temperature with the furnace, removes product surface dust and dirt, makes porous tantalum finished product.
Contriver detects the porous material density of above-mentioned porous tantalum finished product, porosity, aperture and various mechanical property by standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001: its foreign matter content is lower than 0.2%, its even pore distribution, density 13.30g/cm
3, porosity 20%, hole mean diameter 20 μ m, Young's modulus 7.0GPa, unit elongation 14.85%, flexural strength 178MPa, ultimate compression strength 122MPa.This porous tantalum is suitable for substituting the medical embedded material of human body dentale tissue very much.
Embodiment 4: a kind of porous tantalum, it is less than with particle diameter the ta powder that 43 μ m, oxygen level are less than 0.1%, polyvinyl alcohol and sodium bicarbonate powder mix are raw material, then process and make through granulation, injection molding, the demoulding, skimming treatment, vacuum sintering, vacuum annealing.
Wherein, polyvinyl alcohol accounts for 7%, sodium bicarbonate accounts for 20%, ta powder accounts for 73%, in volumn concentration;
Granulation: be that 520 ℃, operating pressure are under 14MPa, described mixed powder to be a granulated into the circular granular of particle diameter 16 μ m in working temperature;
Injection molding and the demoulding: the temperature that described circular granular is injected into mould is that 468 ℃, pressure are 76MPa.Demould time: 8S:
Subsequently mixed powder is put into nonoxidizing atmosphere stove and be warming up to 800 ℃ with certain temperature rise rate, protective atmosphere is that 99.999% argon gas carries out skimming treatment, its before heating up, first pass into pure argon gas at least 30min to get rid of furnace air, temperature control process: the speed with 1.5 ℃/min rises to 400 ℃ from room temperature, insulation 88min, argon gas intake 0.5L/min; Speed with 2.0 ℃/min rises to 800 ℃, insulation 195min, argon gas intake 1L/min from 400 ℃; Powered-down again, the sample furnace cooling after degreasing, argon gas intake 1L/min, until close argon gas while being cooled to room temperature;
For the sample after skimming treatment, with tungsten device, be placed in high vacuum high temperature sintering furnace with certain temperature rise rate intensification vacuum sintering, before heating up, the vacuum tightness of sintering oven at least will reach 10
-4pa, is warming up to 1750 ℃, is incubated 220min, with stove, is chilled to 200～300 ℃ with 16 ℃/min, then is warming up to 1600 ℃, insulation 195min with 13 ℃/min, with 7 ℃/min, is warming up to 2000～2200 ℃, insulation 224min;
Sintering is complete, and vacuum tightness is 10
-3pa, is cooled to 1600 ℃ with the speed of 10～15 ℃/min, insulation 30min; Speed with 12 ℃/min is cooled to 1200 ℃, insulation 60min; Speed with 10 ℃/min is cooled to 800 ℃, then furnace cooling;
For the cooled sample of vacuum sintering, with corundum container, be placed in vacuum annealing furnace and heat up and carry out stress relief annealing processing with certain temperature rise rate, the vacuum tightness before heating up in annealing furnace at least will reach 10
-4pa, is warming up to 800～900 ℃, insulation 385min with 17 ℃/min, then is chilled to 400 ℃, insulation 260min with 3.5 ℃/min, then with 19 ℃/min, is cooled to room temperature, makes medical porous tantalum material.
Contriver detects the porous material density of above-mentioned porous tantalum finished product, porosity, aperture and various mechanical property by standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001: its foreign matter content is lower than 0.2%, its even pore distribution, density 12.87g/cm
3, porosity 23%, hole mean diameter 20 μ m, Young's modulus 6.5GPa, flexural strength 174MPa, ultimate compression strength 123MPa.Through long-term test, this preparation technology's conforming product rate is up to 94.0%.This porous tantalum is suitable for substituting the medical embedded material of human body dentale tissue very much.
In the method providing at above-described embodiment 4, we can also do other selections to wherein each kind of condition can obtain porous tantalum of the present invention equally, below all the other steps with embodiment 4.
The above-mentioned porous tantalum finished product making detects by preceding method, and its foreign matter content can be lower than 0.2%, density reachable 11.67～13.34g/cm
3, porosity can reach 20～30%, and pore diameter can reach 12～25 μ m, Young's modulus can reach that 6.0～7.0Gpa, unit elongation reach 14.0～15.0%, flexural strength can reach 160～180Mpa, ultimate compression strength can reach 115～130Mpa.Make porous tantalum and be applicable to the medical embedded material of human body dentale tissue as an alternative.
Claims (1)
1. the preparation method of a medical porous metal implant material, it is characterized in that: with particle diameter, be less than the ta powder that 43 μ m, oxygen level are less than 0.1%, polyvinyl alcohol and sodium bicarbonate powder mix are raw material, then process through granulation, injection molding, the demoulding, skimming treatment, vacuum sintering, vacuum annealing;
Wherein, polyvinyl alcohol accounts for 7%, sodium bicarbonate accounts for 20%, ta powder accounts for 73%, in volumn concentration;
Granulation: be that 520 ℃, operating pressure are approximately the circular granular that under 14MPa, described mixed powder is a granulated into particle diameter 16 μ m in working temperature;
Injection molding and the demoulding: the temperature that described circular granular is injected into mould is that 468 ℃, pressure are 76Mpa, demould time: 8S;
Subsequently mixed powder is put into nonoxidizing atmosphere stove and be warming up to 800 ℃, protective atmosphere is that 99.999% argon gas carries out skimming treatment, its before heating up, first pass into pure argon gas at least 30min to get rid of furnace air, temperature control process: the speed with 1.5 ℃/min rises to 400 ℃ from room temperature, insulation 88min, argon gas intake 0.5L/min; Speed with 2.0 ℃/min rises to 800 ℃, insulation 195min, argon gas intake 1L/min from 400 ℃; Powered-down again, the sample furnace cooling after degreasing, argon gas intake 1L/min, until close argon gas while being cooled to room temperature;
For the sample after skimming treatment, with tungsten device, be placed in the vacuum sintering that heats up in high vacuum high temperature sintering furnace, before heating up, the vacuum tightness of sintering oven at least will reach 10
-4pa, is warming up to 1750 ℃, is incubated 220min, with stove, is chilled to 200～300 ℃ with 16 ℃/min, then is warming up to 1600 ℃, insulation 195min with 13 ℃/min, with 7 ℃/min, is warming up to 2000～2200 ℃, insulation 224min;
Sintering is complete, and vacuum tightness is 10
-3pa, is cooled to 1600 ℃ with the speed of 10～15 ℃/min, insulation 30min; Speed with 12 ℃/min is cooled to 1200 ℃, insulation 60min; Speed with 10 ℃/min is cooled to 800 ℃, then furnace cooling;
For the cooled sample of vacuum sintering, with corundum container, be placed in vacuum annealing furnace intensification and carry out stress relief annealing processing, the vacuum tightness before heating up in annealing furnace at least will reach 10
-4pa, is warming up to 800～900 ℃, insulation 385min with 17 ℃/min, then is chilled to 400 ℃, insulation 260min with 3.5 ℃/min, then with 19 ℃/min, is cooled to room temperature, makes medical porous tantalum material.
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Cited By (4)
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|---|---|---|---|---|
| CN104674045A (en) * | 2015-02-15 | 2015-06-03 | 北京航空航天大学 | Nanometer porous silver alloy material and preparation method thereof |
| CN105855553A (en) * | 2016-03-30 | 2016-08-17 | 山东省立医院 | Preparation method of porous tantalum material for mouth cavity implantation |
| CN106521219A (en) * | 2017-01-05 | 2017-03-22 | 重庆大学 | Preparation method for TiC particle reinforced titanium-based porous material |
| GB2551755B (en) * | 2016-06-29 | 2019-06-12 | Versarien Plc | A method of manufacturing granules having a layer of metallic particles surrounding a salt core |
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| CN101660076A (en) * | 2009-10-14 | 2010-03-03 | 北京师范大学 | Macro mesh structural porous tantalum prepared by dipping and sintering organic foams |
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| US4059442A (en) * | 1976-08-09 | 1977-11-22 | Sprague Electric Company | Method for making a porous tantalum pellet |
| CN101660076A (en) * | 2009-10-14 | 2010-03-03 | 北京师范大学 | Macro mesh structural porous tantalum prepared by dipping and sintering organic foams |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104674045A (en) * | 2015-02-15 | 2015-06-03 | 北京航空航天大学 | Nanometer porous silver alloy material and preparation method thereof |
| CN105855553A (en) * | 2016-03-30 | 2016-08-17 | 山东省立医院 | Preparation method of porous tantalum material for mouth cavity implantation |
| CN105855553B (en) * | 2016-03-30 | 2018-01-23 | 山东省立医院 | A kind of preparation method of porous tantalum material for oral cavity implantation |
| GB2551755B (en) * | 2016-06-29 | 2019-06-12 | Versarien Plc | A method of manufacturing granules having a layer of metallic particles surrounding a salt core |
| CN106521219A (en) * | 2017-01-05 | 2017-03-22 | 重庆大学 | Preparation method for TiC particle reinforced titanium-based porous material |
| CN106521219B (en) * | 2017-01-05 | 2018-07-03 | 重庆大学 | A kind of preparation method of TiC granule intensified titaniums based porous materials |
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| CN103740964B (en) | 2015-04-08 |
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