CN104940991B - A kind of medical porous tantalum material for substituting dentale and preparation method thereof - Google Patents
A kind of medical porous tantalum material for substituting dentale and preparation method thereof Download PDFInfo
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- CN104940991B CN104940991B CN201510415672.3A CN201510415672A CN104940991B CN 104940991 B CN104940991 B CN 104940991B CN 201510415672 A CN201510415672 A CN 201510415672A CN 104940991 B CN104940991 B CN 104940991B
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 72
- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 52
- 239000011812 mixed powder Substances 0.000 claims abstract description 27
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 25
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 238000007493 shaping process Methods 0.000 claims abstract description 10
- 238000005238 degreasing Methods 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 44
- 238000010438 heat treatment Methods 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 22
- 238000009413 insulation Methods 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 19
- 238000010792 warming Methods 0.000 claims description 18
- 239000011496 polyurethane foam Substances 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 150000002085 enols Chemical class 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000007723 die pressing method Methods 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 38
- 239000011148 porous material Substances 0.000 abstract description 27
- 238000005452 bending Methods 0.000 abstract description 12
- 230000006835 compression Effects 0.000 abstract description 12
- 238000007906 compression Methods 0.000 abstract description 12
- 239000012535 impurity Substances 0.000 abstract description 12
- 239000006261 foam material Substances 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 4
- 238000005299 abrasion Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000000137 annealing Methods 0.000 description 20
- 229910052751 metal Inorganic materials 0.000 description 16
- 239000002184 metal Substances 0.000 description 16
- 229920005830 Polyurethane Foam Polymers 0.000 description 12
- 238000002791 soaking Methods 0.000 description 12
- 210000000988 bone and bone Anatomy 0.000 description 7
- 238000001746 injection moulding Methods 0.000 description 7
- 238000012805 post-processing Methods 0.000 description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- 238000011049 filling Methods 0.000 description 6
- 150000002739 metals Chemical class 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 6
- 229910052721 tungsten Inorganic materials 0.000 description 6
- 239000010937 tungsten Substances 0.000 description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 5
- 239000011261 inert gas Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 238000002513 implantation Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 230000035882 stress Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000006262 metallic foam Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000017074 necrotic cell death Effects 0.000 description 2
- 230000011164 ossification Effects 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QBUKAFSEUHGMMX-MTJSOVHGSA-N (5z)-5-[[3-(1-hydroxyethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical compound C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1C(C)O QBUKAFSEUHGMMX-MTJSOVHGSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000008468 bone growth Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000001149 cognitive effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- 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
- 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
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Dermatology (AREA)
- Medicinal Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Transplantation (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Materials For Medical Uses (AREA)
Abstract
A kind of medical porous tantalum material and preparation method thereof for substituting dentale, mixed-powder is mixed into by tantalum powder and polyvinyl alcohol, sodium acid carbonate, then the mixed-powder is pressed into shaping in Organic Foam Material, degreasing, sintering, cooling and obtained in being heat-treated；The compressing pressure for using is 50~100Mpa, and the medical porous tantalum material pore diameter of formation is 30~50 μm, and porosity is between 30~38%.Porous tantalum preparation method of the present invention employs pure physical abrasion method so that the content of impurity is extremely low in final porous tantalum material, is effectively improved biocompatibility and biological safety；Can be less than 0.2%, density up to 10.34~11.67g/cm by testing its impurity content3, up to 30~38%, pore diameter is up to 30~50 μm for porosity；Elastic modelling quantity up to 4.5~6.0Gpa, bending strength up to 120~130Mpa, compression strength up to 100~140Mpa, porous tantalum of the present invention be highly suitable for substitute dentale medical embedded material.
Description
The present patent application is application number 201110296545.8, the applying date 2011 year 09 month 29 days, and denomination of invention " replace by one kind
The divisional application of medical porous tantalum material for dentale and preparation method thereof ".
Technical field
It is more particularly to a kind of to substitute densification the present invention relates to a kind of porous medical metal implanted material and preparation method thereof
Medical embedded porous tantalum material of bone tissue and preparation method thereof.
Background technology
Porous medical metal implanted material has treatment bone tissue wound, bone formation necrosis and substitutes fine and close bone tissue such as
The important and special purposes such as dentale, existing common this kind of material has porous metals stainless steel, porous metals titanium etc..As bone group
The porous implantation material that wound and bone formation necrosis therapeutic are used is knitted, its porosity should be up to 30~80%, and hole is best
All connect and be uniformly distributed, or the bone growth being allowed to as needed both with human body is consistent, and material is alleviated again in itself
Weight, be adapted to human body implantation use.
And refractory metals tantalum, because it has outstanding biocompatibility, its porous material is expected to foregoing etc. as an alternative
Conventional medical metallic biomaterial.Due to metal tantalum to human body it is harmless, nontoxic, have no side effect, and with domestic and international medical science
Develop rapidly, to tantalum as body implanting material it is cognitive further deeply, people are to human body implantation porous metals tantalum material
The demand of material becomes more and more urgent, requires it also more and more higher.Wherein as porous medical embedded metal tantalum, if can have
There is the physical and mechanical properties for being uniformly distributed interconnected pore and being adapted with human body very high, then it is expected to as a kind of new
Bone tissue alternative materials.
Substantially burnt with powder like that as porous metal material of the medical embedded porous metal material just as
Connection is main processing method, and powder is used with equally distributed porous metal foam structure especially for porosity communication is obtained
To re-sinter abbreviation foam impregnation method in the majority for drying after the dipping of metal dust slurry in sintering process on Organic Foam Material.On
Powder sintered obtained porous metal material generally its Metal Mechanic Property be not it is fine, its main cause be in technique such as
What arrange support and the elimination relation of pore-forming medium, it is metal powder sintered during collapse problem.And known document report
In without good solution and let alone nature.
The document report for making porous tantalum using metal powder sintered legal system is little, is particularly used with obtaining medical embedded material
For the purpose of porous tantalum powder sintering document report almost do not have.That may be referred to is Publication No. CN200510032174,
Title " three-dimensional through hole or some perforations are connected with each other porous metal foam and preparation method thereof " and CN200710152394, name
Claim " a kind of porous foam tungsten and preparation method thereof ".But its porous metals for being obtained or be that filtering material is used, or
It is that Aero-Space and other high temperature applicationss are used with rather than as medical metal implanted material to be, furthermore the porous metals processed
Also non-porous tantalum.
On porous tantalum, US5282861 discloses a kind of cancellous bone implants, cell and tissue receptor of being applied to and opens
Hole tantalum material and its preparation.This porous tantalum is made up of pure business tantalum, and it carries out the carbon that thermal degradation is obtained with polyurethane precursor
Skeleton is support, and the carbon skeleton is in multiple dodecahedron, is grid spline structure in it, integrally spreads all over micropore, and porosity can be high
Up to 98%, then the pure tantalum of business is attached on carbon skeleton by the method for chemical vapour deposition, infiltration micro- to form porous metals
Structure, referred to as chemical deposition.The tantalum layer thickness on porous its surface of tantalum material that this method is obtained 40~60 μm it
Between；In whole porous material, tantalum is weighed about and accounts for 99%, and carbon skeleton weight then accounts for 1% or so.Document further states that this is more
50~the 70MPa of compression strength of Porous materials, 2.5~3.5GPa of elastic modelling quantity, tensile strength 63MPa, amount of plastic deformation 15%.But
Be using it as the medical embedded materials such as fine and close bone tissue such as dentale porous tantalum, it is the mechanical property such as ductility of its material, anti-
Compressive Strength, bending strength etc. have obvious weak point, and influence whether the follow-up processing to porous tantalum material in itself, for example
Cutting of profiled member etc..The same product obtained in foregoing metal powder sintered method also exists such not enough.
The content of the invention
It is an object of the invention to provide a kind of medical porous tantalum material suitable for substituting dentale of good biocompatibility.
Preparation method another object of the present invention is to provide above-mentioned porous tantalum medical material.
The purpose of the present invention is realized by following technological means：
A kind of medical porous tantalum material for substituting dentale, it is characterised in that：Mixed with polyvinyl alcohol, sodium acid carbonate by tantalum powder
It is obtained into mixed-powder, then repressed shaping, degreasing, sintering, cooling and heat treatment；It is described it is compressing be will be described mixed
Close powder to be pressed into Organic Foam Material, its pressure is 50~100Mpa, and the medical porous tantalum material pore diameter of formation is 30
~50 μm, porosity is between 30~38%.
In the R＆D process of medical porous tantalum material, syntheti c route is numerous, but inventor creatively proposes use
Fine and close medical porous tantalum implantation material prepared by above-mentioned processing step, can be less than 0.2%, its biology by testing its impurity content
Compatibility is good with biological safety, and density is up to 10.34~11.67g/cm3, up to 30~38%, pore diameter can for porosity
Up to 30~50 μm；Elastic modelling quantity up to 4.5~6.0Gpa, bending strength up to 120~130Mpa, compression strength up to 100~
140Mpa, porous tantalum of the present invention is highly suitable for substituting the medical embedded material of dentale.
The average grain diameter of the Ta powder that the present invention is used is less than 0.1% less than 43 microns, oxygen content, is commercially available prod；
Above-mentioned polyvinyl alcohol, sodium acid carbonate are also commercially available prod.Above-mentioned polyvinyl alcohol mainly plays shaping but it is also equipped with simultaneously
The effect of pore-creating, above-mentioned sodium acid carbonate plays pore-creating.It is 10 that vacuum environment of the present invention preferably uses vacuum-4Pa~10- 3The vacuum condition of Pa.The above-mentioned preferred polyurethane foam of Organic Foam Material, more preferably 0.48~0.89mm of aperture, density
0.015g/cm3~0.035g/cm3, more than 50 °, (most preferably aperture is 0.56~0.72mm, density 0.025g/cm to hardness3, firmly
Degree 50 °~80 °) polyurethane foam in.
The inventor in R＆D process further study show that, if controlled in above-mentioned preparation it is bad, though as above institute can be obtained
State be suitable for substitute dentale medical embedded material but product percent of pass is not high：Such as powder pressing forming hardly possible, after pressing portion
Point easily occur layering, it is uneven, there are the technical problems such as crackle in degreasing rear portion branch.
In order that shaping is easier in powder compaction process, so as to improve yield rate, finished product hole uniformity, make to prepare
Journey is more stable, and the consumption of polyvinyl alcohol is that the consumption of 5~10%, sodium acid carbonate is 20~30%, surplus in above-mentioned mixed-powder
It is tantalum powder, (in terms of volumn concentration is directly calculated by the situation of final porous tantalum material in terms of volumn concentration
Unit, the density according further to respective substance in the weighing of above-mentioned mixed-powder calculates its corresponding quality weighing), enter one
Step preferably polyvinyl alcohol accounts for 7~9%, sodium acid carbonate and accounts for 26~29%, balance of tantalum powder；It is above-mentioned it is compressing during pressure
Power is preferably 70~80Mpa.
In order that idiosome is more stable in skimming processes, reduction easily appearance part idiosome deforms, aperture is uneven, so as to enter
One step improves yield rate, quality stability, and above-mentioned skimming processes are progressively warming up to the speed of 0.5 DEG C/min~3 DEG C/min
400~800 DEG C, it is passed through with argon gas and is constituted protective atmosphere and be incubated 60min~240min；Further preferably with 2.5~3 DEG C/min
Speed be progressively warming up to 400~800 DEG C, be passed through with argon gas and constituted protective atmosphere and be incubated 150min~240min.
The preparation method of the medical porous tantalum material of above-mentioned replacement dentale, is formed using die pressing sintering, and its feature is
Mixed powder is mixed into tantalum powder and polyvinyl alcohol, sodium bicarbonate powder, the consumption of wherein polyvinyl alcohol accounts for 5~10%, bicarbonate
The consumption of sodium accounts for 20~30%, balance of tantalum powder, in terms of volumn concentration；Again by the mixed-powder under 50~100Mpa
Shaping, degreasing, vacuum-sintering, cooling and heat treatment are obtained porous tantalum material in being pressed into Organic Foam Material.
The average grain diameter of above-mentioned raw materials tantalum powder is less than 0.1% less than 43 microns, oxygen content；Above-mentioned mixed powder is preferably poly- second
Enol accounts for 7~9%, sodium acid carbonate and accounts for 26~29%, balance of tantalum powder, still more preferably for polyvinyl alcohol accounts for 8%, bicarbonate
Sodium accounts for 27%, balance of tantalum powder, in terms of volumn concentration.The above-mentioned preferred polyurethane foam of Organic Foam Material, further preferably
It is 0.48~0.89mm of aperture, density 0.015g/cm3~0.035g/cm3, hardness more than 50 ° (most preferably aperture be 0.56~
0.72mm, density 0.025g/cm3, 50 °~80 ° of hardness) polyurethane foam in.
In order that pressing pressure is uniform, not stratified during compacting embryo processed, so that final porous tantalum distribution of pores is more equal
Even, quality is more stable, and the pressure used in above-mentioned pressing process is preferably 70~80Mpa；In above-mentioned skimming processes be preferably with
The speed of 0.5 DEG C/min~3 DEG C/min is progressively warming up to 400~800 DEG C, is passed through with argon gas and is constituted protective atmosphere and be incubated
60min~240min, is further preferably progressively warming up to 400~800 DEG C with the speed of 2.5~3 DEG C/min, and structure is passed through with argon gas
Into protective atmosphere and 150min~240min is incubated, still more preferably 400 are progressively warming up to the speed of 2.5 DEG C/min~
800 DEG C, it is passed through with argon gas and is constituted protective atmosphere and be incubated 220min.
The further feature of another aspect of the present invention is：10 are not less than in vacuum-4~10-3Pa, temperature 2000~
2200 DEG C, the soaking time vacuum-sintering of 1~5 hour treatment is obtained porous sintered body.Sintering process can fill inertia when being incubated
Gas shield replaces vacuum protection；Vacuum annealing treatment is finally carried out, wherein vacuum annealing treatment refers to by after vacuum-sintering
Continue keeping temperature be in 1000~1250 DEG C, soaking time 1~4 hour, vacuum is not less than 10-4~10-3Pa。
Vacuum-sintering condition is also included：Vacuum is not less than 10-3Pa, with the heating rate of 10~20 DEG C/min from room temperature
Rise to 1200 DEG C~1500 DEG C, after insulation 1h~2h；2000~2200 DEG C are warming up to the heating rate less than 20 DEG C/min again,
At least it is incubated 2h~4h.
Cooling condition after vacuum-sintering is also included：Vacuum is not less than 10-3Pa is not low to be not higher than 25 DEG C/min
Cooldown rate mode is gradually dropped in 10 DEG C/min, cooling down to 800 DEG C, each section of soaking time 30min is segmented to sintered porous bodies
~90min, then cools to normal temperature with the furnace.
Vacuum annealing condition is also included：Vacuum is not less than 10-4Pa, 1000 are risen to the speed for being not higher than 30 DEG C/min
~1250 DEG C, it is incubated 4h~6h；It is segmented with the first slow rear fast cooldown rate to be not less than 5 DEG C/min but not higher than 30 DEG C/min again
Room temperature is cooled to, each section of soaking time tapers off and selected no more than in 1.5h~3h.
On this basis further the characteristics of is：The ungrease treatment condition is also included：Progressively it is warming up to 600~
800 DEG C, composition protective atmosphere specifically is passed through with pure argon gas (99.9999%), with the speed of 1~3 DEG C/min from room temperature liter
To 400 DEG C, 60~120min is incubated, 600~800 DEG C are risen to from 400 DEG C with the speed of 1.5~2.5 DEG C/min, insulation 180~
240min；The vacuum-sintering condition is also included：1200~1250 DEG C are risen to from room temperature with the speed of 10~15 DEG C/min, is protected
30~60min of temperature, vacuum is 10-4Pa~10-3Pa；1500 DEG C are risen to the speed of 10~20 DEG C/min, insulation 30~
60min, vacuum is 10-4Pa~10-3Pa, 2000~2200 DEG C are risen to the speed of 6~20 DEG C/min, and insulation 120~
240min, vacuum is 10-4Pa~10-3Pa；Cooling condition after vacuum-sintering is also included：Vacuum is 10-4Pa~10- 3Pa；1500~1600 DEG C are cooled to the speed of 10~20 DEG C/min, 30~60min is incubated；With the speed of 12~20 DEG C/min
1200~1250 DEG C are cooled to, 60~90min is incubated；800 DEG C are cooled to the speed of 10~20 DEG C/min, it is then cold with stove
But；The vacuum annealing condition is also included：1000~1250 DEG C are risen to the speed of 15~30 DEG C/min, insulation 240~
480min, vacuum is 10-4Pa~10-3Pa, then it is cooled to 1000 DEG C with the speed of 5~10 DEG C/min, insulation 90~
180min, vacuum is 10-4Pa~10-3Pa；800 DEG C are cooled to the speed of 10~20 DEG C/min, 60~120min is incubated,
Vacuum is 10-4Pa；Room temperature is cooled to the speed of 20~30 DEG C/min, vacuum is 10-4Pa~10-3Pa。
Porous tantalum preparation method of the present invention employs pure physical abrasion method so that the content of impurity in final porous tantalum material
It is extremely low, it is effectively improved biocompatibility and biological safety；To compressing, degreasing of the invention, sintering and annealing steps
Optimization of process conditions so that high yield rate, finished product aperture uniformity more preferably, make that preparation process is more stable, quality stability is good,
Effectively eliminate thermal stress, make porous tantalum materials microstructure evenly, further to improve the mechanical property of porous tantalum as by force
Degree, toughness are all improved simultaneously, and preparation technology of the present invention causes that product qualified rate is high, produces stabilization, and product percent of pass can be high
Up to 95%.Obtained porous tantalum finished product even pore distribution of the invention and connection, good biocompatibility, contain by testing its impurity
Amount can be less than 0.2%, density up to 10.34~11.67g/cm3, up to 30~38%, pore diameter is up to 30~50 for porosity
μm；Elastic modelling quantity is up to 4.5~6.0Gpa, bending strength up to 120~130Mpa, compression strength up to 100~140Mpa, sheet
Invention porous tantalum is highly suitable for substituting the medical embedded material of dentale.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that be that following examples are only used
It is further described in the present invention, it is impossible to be interpreted as limiting the scope of the invention, person skilled in art can
Some nonessential modifications and adaptations are made to the present invention with according to the invention described above content.
A kind of medical porous tantalum material for substituting dentale is specifically selection polyvinyl alcohol for forming agent, sodium acid carbonate are pore-creating
Agent, mixed powder is mixed into average grain diameter less than 43 microns, tantalum powder of the oxygen content less than 0.1%, will be mixed under 50~100Mpa
Close during powder is pressed into Organic Foam Material and be molded, then obtained through degreasing, sintering, cooling and heat treatment.The porous tantalum of formation is through inspection
Gaging hole porosity is between 30~38%, 30~50 μm of pore diameter.
More specifically, above-mentioned porous tantalum is by polyvinyl alcohol, 20~30% of 5~10% (in terms of volumn concentrations)
The sodium acid carbonate of (in terms of volumn concentration) and the tantalum powder of surplus are mixed into mixed powder, put it into injection moulding machine plus
It is pressed into shaping in polyurethane foam；It is placed in again in tungsten device and is put into the protection gas that pure argon gas (99.9999%) are passed through composition
Uniform temperature is progressively warming up in atmosphere stove, and insulation carries out ungrease treatment to remove pore creating material, forming agent and polyurethane foam, its
In argon gas was first passed through before intensification to exclude furnace air, the sample furnace cooling after degreasing；For the sample after ungrease treatment
Product are placed in tungsten device and 2000~2200 DEG C are progressively warming up in high vacuum high temperature sintering furnace, and soaking time carries out vacuum in 1~5 hour
Sintering, the vacuum of sintering furnace will at least reach proper level before intensification, the sample furnace cooling after vacuum-sintering, cooling
During keep certain vacuum or by certain cooldown rate sub-sectional cooling to keep uniform temperature in reasonable time,
Can be using filling with inert gas as protective atmosphere in insulating process.Sample after being cooled down for vacuum-sintering is put with corundum container
Progressively heated up in vacuum annealing furnace, insulation carries out stress relief annealing process, the holding before intensification in annealing furnace is certain
Vacuum, the sample furnace cooling after vacuum annealing treatment also keeps certain vacuum or by certain cold in cooling procedure
But speed sub-sectional cooling, can be using filling with inert gas as guarantor in insulating process to keep uniform temperature in reasonable time
Shield atmosphere, finally carries out conventional post processing and porous tantalum is obtained.
To be placed in tungsten crucible to be put into atmosphere furnace to be heated up with certain heating rate for ungrease treatment, its
Argon gas or other inert gases are first passed through before intensification to exclude furnace air, temperature control process is with suitable heating rate from room
Temperature rise is to certain temperature, insulation, then heats up, is incubated.Vacuum-sintering treatment is carried out for the sample after ungrease treatment, is by it
The maximum sintering temperature for being warming up to tantalum with certain heating rate is placed in high vacuum high temperature sintering furnace with tungsten device carries out vacuum burning
Knot, sintering furnace keeps certain vacuum before intensification, and such as 1200 DEG C~1250 DEG C are warming up to certain heating rate,
Insulation, keeps vacuum；Such as 1250 DEG C~1500 DEG C are warming up to again with certain heating rate, are incubated, then with certain intensification
Speed is warming up to the maximum sintering temperature of such as tantalum, insulation, holding vacuum；Sintering is finished, and keeps vacuum, with certain cooling speed
Rate is cooled to such as 1500 DEG C~1600 DEG C, is incubated, then is cooled to such as 1200 DEG C~1250 DEG C with certain rate of temperature fall, protects
Temperature, is also cooled to such as 800 DEG C, then furnace cooling with certain rate of temperature fall.Sample after being cooled down for vacuum-sintering enters
Row vacuum annealing is processed, and is to be placed in vacuum annealing furnace it with corundum container to be warming up to such as 1000 with certain heating rate
DEG C~1250 DEG C carry out stress relief annealing process, the holding vacuum before intensification in annealing furnace, with certain heating rate
1000 DEG C~1250 DEG C are risen to from room temperature, insulation keeps vacuum；Such as 1000 DEG C are cooled to certain rate of temperature fall again, are protected
Temperature；Such as 800 DEG C, insulation are cooled to certain rate of temperature fall again；Room temperature is also cooled down with certain rate of temperature fall.Finally carry out
Conventional post processing is obtained porous tantalum.
Inventor uses metal powder sintered method main based on physical abrasion method, has done substantial amounts of theory analysis and experiment
Checking, obtaining porous tantalum product can be less than 0.2%, density up to 10.34~11.67g/cm by testing its impurity content3, hole
, up to 30~38%, pore diameter is up to 30~50 μm for porosity；Elastic modelling quantity is up to 4.5~6.0Gpa, bending strength up to 120
~130Mpa, compression strength are up to 100~140Mpa.
Embodiment 1：Weigh the tantalum powder and bicarbonate of polyvinyl alcohol, average grain diameter less than 43 microns of oxygen contents less than 0.1%
Sodium is mixed into mixed-powder, and wherein polyvinyl alcohol accounts for 8%, sodium acid carbonate and accounts for 27%, tantalum powder and accounts for 65%, with volume basis
Content meter.Extrusion forming：Above-mentioned mixed-powder is pressed into polyurethane foam (aperture in injection moulding machine under 80Mpa
0.48~0.89mm, density 0.015g/cm3~0.035g/cm3, hardness is more than 50 °) and middle shaping.Ungrease treatment：Vacuum 10- 4Pa, with the heating rate of 2.5 DEG C/min from room temperature to 400 DEG C, insulation 100min；Again with the heating rate of 2 DEG C/min from
400 DEG C are warming up to 700 DEG C, soaking time 220 minutes.Vacuum-sintering：Sinter in a vacuum furnace, 2000 DEG C of sintering temperature, insulation 2
Hour, vacuum 10-4Pa, sintering process argon filling gas shielded removes surface dirt and dirt after taking out product, and obtained sample is again
Carry out conventional post-processing to obtain porous tantalum finished product.
Inventor press the standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001 to above-mentioned porous tantalum into
The porous material density of product, porosity, aperture and various mechanical properties are detected：Its impurity content is less than 0.2%, its hole
It is evenly distributed, density 10.84g/cm3, porosity 35%, 30 μm of pore mean diameters, elastic modelling quantity 5.5GPa, bending strength
130MPa, compression strength 140MPa.
Embodiment 2：Weigh the tantalum powder and bicarbonate of polyvinyl alcohol, average grain diameter less than 43 microns of oxygen contents less than 0.1%
Sodium is mixed into mixed-powder, and wherein polyvinyl alcohol accounts for 6%, sodium acid carbonate and accounts for 29%, tantalum powder and accounts for 65%, with volume basis
Content meter.Extrusion forming：Will above-mentioned mixed-powder add be pressed under 70Mpa in injection moulding machine aperture for 0.56~
0.72mm, density 0.025g/cm3, it is molded in the polyurethane foam that 50 °~80 ° of hardness.Ungrease treatment：Vacuum 10-4Pa, with 1
DEG C/heating rate of min is from room temperature to 400 DEG C, insulation 60min；Risen from 400 DEG C with the heating rate of 2.5 DEG C/min again
Temperature is to 800 DEG C, soaking time 180 minutes.Vacuum-sintering：Sinter in a vacuum furnace, 2100 DEG C of sintering temperature, be incubated 4 hours, very
Reciprocal of duty cycle 10-4Pa, sintering process argon filling gas shielded removes surface dirt and dirt after taking out product, and obtained sample is carried out often again
Rule post-process to obtain porous tantalum finished product.
Inventor press the standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001 to above-mentioned porous tantalum into
The porous material density of product, porosity, aperture and various mechanical properties are detected：Its impurity content is less than 0.2%, its hole
It is evenly distributed, density 10.34g/cm3, porosity 38%, 32 μm of pore mean diameters, elastic modelling quantity 4.5GPa, bending strength
123MPa, compression strength 110MPa.
Embodiment 3：Weigh the tantalum powder and bicarbonate of polyvinyl alcohol, average grain diameter less than 43 microns of oxygen contents less than 0.1%
Sodium is mixed into mixed-powder, and wherein polyvinyl alcohol accounts for 10%, sodium acid carbonate and accounts for 23%, tantalum powder and accounts for 67%, with volume hundred
Divide content meter.Extrusion forming：Will above-mentioned mixed-powder add be pressed under 52Mpa in injection moulding machine aperture for 0.56~
0.72mm, density 0.025g/cm3, it is molded in the polyurethane foam that 50 °~80 ° of hardness.Ungrease treatment：Vacuum 10-4Pa, with 3
DEG C/heating rate of min is from room temperature to 400 DEG C, insulation 120min；Risen from 400 DEG C with the heating rate of 1.5 DEG C/min again
Temperature is to 750 DEG C, soaking time 240 minutes.Vacuum-sintering：Sinter in a vacuum furnace, 2200 DEG C of sintering temperature, be incubated 2.5 hours,
Vacuum 10-3Pa, sintering process argon filling gas shielded, cooling is come out of the stove, and removes product surface dust and dirt, and obtained sample enters again
Row it is conventional post-process to obtain porous tantalum finished product.
Inventor press the standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001 to above-mentioned porous tantalum into
The porous material density of product, porosity, aperture and various mechanical properties are detected：Its impurity content is less than 0.2%, its hole
It is evenly distributed, density 10.67g/cm3, porosity 36%, 34 μm of pore mean diameters, elastic modelling quantity 6.0GPa, bending strength
128MPa, compression strength 100MPa.
Embodiment 4：Weigh the tantalum powder and bicarbonate of polyvinyl alcohol, average grain diameter less than 43 microns of oxygen contents less than 0.1%
Sodium is mixed into mixed-powder, and wherein polyvinyl alcohol accounts for 5%, sodium acid carbonate and accounts for 30%, tantalum powder and accounts for 65%, with volume basis
Content meter.Extrusion forming：Will above-mentioned mixed-powder add be pressed under 96Mpa in injection moulding machine aperture for 0.56~
0.72mm, density 0.025g/cm3, it is molded in the polyurethane foam that 50 °~80 ° of hardness.Ungrease treatment：Vacuum 10-4Pa, with 2
DEG C/heating rate of min is from room temperature to 400 DEG C, insulation 80min；Risen from 400 DEG C with the heating rate of 1.5 DEG C/min again
Temperature is to 800 DEG C, soaking time 190 minutes.Vacuum-sintering：Sinter in a vacuum furnace, 2150 DEG C of sintering temperature, be incubated 2 hours, very
Reciprocal of duty cycle 10-4Pa, sintering process argon filling gas shielded, cooling is come out of the stove, and removes product surface dust and dirt, and obtained sample is carried out again
Conventional post-processes to obtain porous tantalum finished product.
Inventor press the standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001 to above-mentioned porous tantalum into
The porous material density of product, porosity, aperture and various mechanical properties are detected：Its impurity content is less than 0.2%, its hole
It is evenly distributed, density 11.17g/cm3, porosity 33%, 40 μm of pore mean diameters, elastic modelling quantity 4.5GPa, bending strength
120MPa, compression strength 135MPa.
Embodiment 5：A kind of porous tantalum, it is with particle diameter less than 43 μm, ta powder of the oxygen content less than 0.1%, polyethylene
Alcohol and sodium acid carbonate mixed powder are raw material, then repressed shaping, ungrease treatment, vacuum-sintering, vacuum annealing and conventional post processing
It is obtained.
Wherein, polyvinyl alcohol accounts for 7%, sodium acid carbonate and accounts for 20%, ta powder and accounts for 73%, in terms of volumn concentration；
It is compressing：Will raw material mixed powder end add be pressed under 65Mpa in injection moulding machine aperture for 0.56~
0.72mm, density 0.025g/cm3, it is molded in the polyurethane foam that 50 °~80 ° of hardness；
Ungrease treatment：Under inert gas shielding atmosphere or vacuum 10-4~10-3Pa, is warming up to 2.5~3 DEG C/min
400 DEG C~800 DEG C, with argon gas as protective atmosphere, soaking time 150~240 minutes to be removing polyvinyl alcohol therein and carbonic acid
Hydrogen sodium；
Vacuum-sintering：Vacuum is less than 10-4Pa~10-3Pa, 2000~2200 DEG C of temperature, soaking time 1~5 hour is burnt
Applying argon gas or other inert gas shieldings when knot process is incubated, to obtain porous material；
Vacuum annealing：By the follow-up continuous keeping temperature of vacuum-sintering be in 1000~1250 DEG C, soaking time 1~4 hour,
Vacuum is 10-4~10-3Pa, to carry out stress relief annealing process；Obtained sample carries out conventional post-processing to obtain porous tantalum again
Finished product.
Inventor press the standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001 to above-mentioned porous tantalum into
The porous material density of product, porosity, aperture and various mechanical properties are detected：Its impurity content is less than 0.2%, its hole
It is evenly distributed, density 10.34g/cm3, porosity 38%, 39 μm of pore mean diameters, elastic modelling quantity 4.9GPa, bending strength
122MPa, compression strength 134MPa.
Embodiment 6：A kind of porous tantalum, it is with particle diameter less than 43 μm, ta powder of the oxygen content less than 0.1%, polyethylene
Alcohol and sodium acid carbonate mixed powder are raw material, then repressed shaping, ungrease treatment, vacuum-sintering, vacuum annealing and conventional post processing
It is obtained.
Wherein, polyvinyl alcohol accounts for 7%, sodium acid carbonate and accounts for 20%, ta powder and accounts for 73%, in terms of volumn concentration；
It is compressing：Will raw material mixed powder end add be pressed under 65Mpa in injection moulding machine aperture for 0.56~
0.72mm, density 0.025g/cm3, it is molded in the polyurethane foam that 50 °~80 ° of hardness；
Mixed-powder is put into nonoxidizing atmosphere stove after compressing is warming up to 800 DEG C with certain heating rate, protected
Shield atmosphere carries out ungrease treatment for 99.999% argon gas, and it was first passed through pure argon gas at least 30min to exclude stove before intensification
Interior air, temperature control process：400 DEG C are risen to from room temperature with the speed of 1.5 DEG C/min, 88min, argon gas intake 0.5L/ is incubated
min；800 DEG C are risen to from 400 DEG C with the speed of 2.0 DEG C/min, 195min, argon gas intake 1L/min is incubated；Turn off power supply,
Sample furnace cooling after degreasing, argon gas intake 1L/min, until closing argon gas when being cooled to room temperature；
It is placed in high vacuum high temperature sintering furnace with tungsten device for the sample after ungrease treatment and is heated up with certain heating rate
Vacuum-sintering is carried out to 2200 DEG C, the vacuum of sintering furnace will at least reach 10 before intensification-4Pa, with 10~15 DEG C/min's
Speed rises to 1200 DEG C from room temperature, is incubated 30min, and vacuum is 10-4Pa；1500 DEG C, insulation are risen to the speed of 10 DEG C/min
30min, vacuum is 10-4Pa~10-3Pa；2200 DEG C are risen to the speed of 6 DEG C/min, 120min is incubated, vacuum is 10- 3Pa；Sintering is finished, and vacuum is 10-3Pa, 1600 DEG C are cooled to the speed of 10~15 DEG C/min, are incubated 30min；With 12 DEG C/
The speed of min is cooled to 1200 DEG C, is incubated 60min；800 DEG C are cooled to the speed of 10 DEG C/min, then furnace cooling；
Sample after being cooled down for vacuum-sintering is placed in vacuum annealing furnace with certain heating rate liter with corundum container
Warm to 1250 DEG C carry out stress relief annealing process, and the vacuum before intensification in annealing furnace will at least reach 10-4Pa, with 15
DEG C/speed of min rises to 1250 DEG C from room temperature, is incubated 240min, vacuum is 10-4Pa~10-3Pa；Again with the speed of 5 DEG C/min
Rate is cooled to 1000 DEG C, is incubated 180min, and vacuum is 10-4Pa~10-3Pa；800 DEG C are cooled to the speed of 10 DEG C/min,
Insulation 120min, vacuum is 10-4Pa；Room temperature is cooled to the speed of 20 DEG C/min, vacuum is 10-4Pa.Finally carry out often
Rule post processing is obtained porous tantalum.
Inventor press the standards such as GB/T5163-2006, GB/T5249-1985, GB/T6886-2001 to above-mentioned porous tantalum into
The porous material density of product, porosity, aperture and various mechanical properties are detected：Its impurity content is less than 0.2%, its hole
It is evenly distributed, density 11.67g/cm3, porosity 30%, 50 μm of pore mean diameters, elastic modelling quantity 5.8GPa, bending strength
127MPa, compression strength 133MPa.The preparation technology product percent of pass is up to 93.4%.
In the method that above-described embodiment 6 is given, we can also make other same energy of selection to various conditions therein
Obtain porous tantalum of the present invention.
Gained porous tantalum finished product is detected by preceding method：
| Embodiment | 7 | 8 | 9 | 10 | 11 | 12 | 13 |
| 11.34 | 10.34 | 10.67 | 11.67 | 11.17 | 11.0 | 10.50 | |
| Porosity (%) | 32 | 38 | 36 | 30 | 33 | 34 | 37 |
| Aperture (μm) | 44 | 50 | 48 | 35 | 37 | 30 | 40 |
| Elastic modelling quantity (GPa) | 4.7 | 4.3 | 4.9 | 5.8 | 5.5 | 6.0 | 5.2 |
| Bending strength (MPa) | 120 | 122 | 125 | 128 | 124 | 130 | 121 |
| Compression strength (MPa) | 123 | 100 | 115 | 118 | 128 | 140 | 135 |
Claims (4)
1. a kind of medical porous tantalum material for substituting dentale, is formed using die pressing sintering, it is characterised in that：With tantalum powder and poly- second
Enol, sodium bicarbonate powder are mixed into mixed powder, the consumption of wherein polyvinyl alcohol account for 5~10%, sodium acid carbonate consumption account for 20~
30%th, balance of tantalum powder, in terms of volumn concentration；Aperture is pressed under 50~100Mpa again for 0.56~0.72mm, density
0.025g/cm3, hardness 500~800Polyurethane foam in shaping, degreasing, vacuum-sintering, cooling and heat treatment be obtained porous tantalum
Material；
The ungrease treatment condition is：600~800 DEG C are progressively warming up to, are specifically passed through with 99.9999% pure argon gas and are constituted
Protective atmosphere, 400 DEG C are risen to the speed of 1~3 DEG C/min from room temperature, are incubated 60~120min, then with 1.5~2.5 DEG C/min
Speed rise to 600~800 DEG C from 400 DEG C, be incubated 180~240min；
The vacuum-sintering condition is：With the speed of 10~15 DEG C/min 1200~1250 DEG C are risen to from room temperature, insulation 30~
60min, vacuum is 10-4Pa~10-3Pa；1500 DEG C are risen to the speed of 10~20 DEG C/min again, 30~60min is incubated, very
Reciprocal of duty cycle is 10-4Pa~10-3Pa；Then 2000~2200 DEG C are risen to the speed of 6~20 DEG C/min, are incubated 120~240min,
Vacuum is 10-4Pa~10-3Pa；
Cooling condition after vacuum-sintering is：Vacuum is 10-4Pa~10-3Pa；It is cooled to the speed of 10~20 DEG C/min
1500~1600 DEG C, it is incubated 30~60min；Again 1200~1250 DEG C are cooled to the speed of 12~20 DEG C/min, insulation 60~
90min；Then 800 DEG C are cooled to the speed of 10~20 DEG C/min, then furnace cooling；
The heat treatment condition is：1000~1250 DEG C are risen to the speed of 15~30 DEG C/min, 240~480min is incubated, very
Reciprocal of duty cycle is 10-4Pa~10-3Pa, then 1000 DEG C are cooled to the speed of 5~10 DEG C/min, 90~180min is incubated, vacuum is
10-4Pa~10-3Pa；Then 800 DEG C are cooled to the speed of 10~20 DEG C/min, are incubated 60~120min, vacuum is 10- 4Pa；Then room temperature is cooled to the speed of 20~30 DEG C/min, vacuum is 10-4Pa~10-3Pa。
2. the medical porous tantalum material of dentale is substituted as claimed in claim 1, it is characterised in that：Poly- second in the mixed-powder
Enol accounts for 7~9%, sodium acid carbonate and accounts for 26~29%, balance of tantalum powder, in terms of volumn concentration；It is described it is compressing during
Pressure be 70~80Mpa.
3. the medical porous tantalum material of dentale is substituted as claimed in claim 1, it is characterised in that：The Ta powder it is average
Particle diameter is less than 0.1% less than 43 microns, oxygen content；The mixed powder accounts for 26~29% for polyvinyl alcohol accounts for 7~9%, sodium acid carbonate,
Balance of tantalum powder, in terms of volumn concentration.
4. as described in claim 1,2 or 3 replacement dentale medical porous tantalum material, it is characterised in that：The mixed powder is
Polyvinyl alcohol accounts for 8%, sodium acid carbonate and accounts for 27%, balance of tantalum powder, in terms of volumn concentration.
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| CN104940991A (en) | 2015-09-30 |
| WO2013044767A1 (en) | 2013-04-04 |
| CN105056296A (en) | 2015-11-18 |
| CN102793945A (en) | 2012-11-28 |
| CN105056296B (en) | 2018-01-30 |
| CN102793945B (en) | 2015-08-19 |
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Effective date of registration: 20200427 Address after: 400042 Chongqing city Yubei District Qinye Road No. 9 Patentee after: CHONGQING RUNZE PHARMACEUTICAL Co.,Ltd. Address before: Lucheng District of Wenzhou City, Zhejiang province 325000 riverside Street stool Bridge No. 67 building 302 room 5 Patentee before: Zhu Qidong |