CN103740967B - Method for preparing medical porous tantalum implantation material - Google Patents
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- CN103740967B CN103740967B CN201310700107.2A CN201310700107A CN103740967B CN 103740967 B CN103740967 B CN 103740967B CN 201310700107 A CN201310700107 A CN 201310700107A CN 103740967 B CN103740967 B CN 103740967B
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Abstract
The invention relates to a method for preparing a medical porous tantalum implantation material, which comprises the following steps: preparing a polyvinyl alcohol water solution and tantalum powder into slurry, injecting the slurry into organic foam by shake pressurization, drying, degreasing, sintering, cooling and carrying out heat treatment to obtain the medical porous tantalum material. The mass concentration of the polyvinyl alcohol water solution is 2-8%, and the shake frequency is 20-80 times/minute. The heat treatment comprises the following steps: under the vacuum degree of 10<-4>-10<-3>Pa, heating to 800-900 DEG C at the rate of 10-20 DEG C/minute, keeping the temperature for 240-480 minutes, cooling to 400 DEG C at the rate of 2-5 DEG C/minute, keeping the temperature for 120-300 minutes, and carrying out furnace cooling to room temperature. The prepared porous tantalum is very suitable to be used as a medical implantation material as a substitute for bearing bone tissues, and ensures the biocompatibility and mechanical properties. In addition, the reagents, organic foam and the like, which can be wholly decomposed and can not leave residues in the sintering process, are preferably used in the preparation process, thereby being beneficial to ensuring the biosafety of the implantation material.
Description
The present patent application is the divisional application of application number 201110300340.2, the applying date on 09 29th, 2011, denomination of invention " a kind of method preparing medical porous tantalum embedded material ".
Technical field
The present invention relates to a kind of method preparing porous medical metal implanted material, particularly relate to a kind of method preparing the medical porous tantalum embedded material being applicable to alternative load bone tissue.
Background technology
Porous medical metal implanted material has the downright bad and alternative dense bone tissue for the treatment of osseous tissue wound, bone formation purposes as important and special in tooth etc., and showing common this kind of material has porous metal stainless steel, porous metal titanium etc.As the porous embedded material that osseous tissue wound and bone formation necrosis therapeutic use, its porosity should reach 30 ~ 80%, and hole is preferably all communicated with and is uniformly distributed, or make it both consistent with the bone growth of human body as required, alleviate again the weight of material itself, implant with applicable human body and 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, to tantalum going deep into further as body implanting material cognition, the demand of people to human body implantation porous metal tantalum material becomes more and more urgent, 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 being uniformly distributed open pore and adapting with human body, then it is expected to as a kind of novel osseous tissue equivalent material.
As medical embedded porous metal material just as porous metal material be main working method with powder sintering like that substantially, especially obtain porosity communication and equally distributed porous metal foam structure adopt the dipping of the metal-powder slurry in powder sintering on Organic Foam Material after drying reburn and tie that to be called for short foam impregnation method in the majority.About powder sintered obtained porous metal material usually its Metal Mechanic Property be not very well, its major cause how technique arranges the problem of subsiding in the support of pore-forming medium and elimination relation, metal powder sintered process.And all there is no good solution in known bibliographical information and let alone nature.
Adopt metal powder sintered legal system to make the bibliographical information of porous tantalum seldom, particularly almost do not have by the porous tantalum powder sintering bibliographical information obtained for the purpose of medical embedded material use.Can reference be publication number be CN200510032174, title " three-dimensional through hole or some perforations are connected with each other porous metal foam and preparation method thereof " and CN200710152394, title " a kind of porous foam tungsten and preparation method thereof ".But its porous metal obtained or for filtering material use, or share for aerospace and other high-temperature field but not use as medical metal implanted material, moreover the porous metal processed also non-porous tantalum.
About porous tantalum, US5282861 discloses and is a kind ofly applied to cancellous bone implants, the perforate tantalum material of biological cells and tissues susceptor and preparation thereof.This porous tantalum is made up of pure business tantalum, it carries out carbon skeleton that thermal destruction obtains for support with polyurethane precursor, this carbon skeleton is multiple dodecahedron, it is mesh-like structure in it, entirety spreads all over micropore, porosity can up to 98%, then by commercially pure tantalum by the methods combining of chemical vapour deposition, infiltration to carbon skeleton to form porous metal microstructure, referred to as chemical deposition.The tantalum layer thickness on its surface of porous tantalum material that this method obtains is between 40 ~ 60 μm; In whole porous material, tantalum heavily accounts for 99%, and carbon skeleton weight then accounts for about 1%.Document is recorded further, 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 tooth, the mechanical property of its material is obvious weak point as ductility has, and can have influence on the follow-up processing to porous tantalum material itself, the cutting etc. of such as profiled member.Also all there is such deficiency in the product obtained in aforesaid metal powder sintered method equally.
Summary of the invention
The object of the present invention is to provide a kind of method of medical porous tantalum embedded material preparing good biocompatibility, mechanical toughness excellence, simultaneously this preparation method easy and simple to handle, be suitable for commercial scale production.
The object of the invention is to be realized by following technique means:
A kind of method preparing medical porous tantalum embedded material, it is characterized in that: the PVOH aqueous solution and tantalum powder are made into slurry, described slurry is injected Organic Foam Material by vibrations pressurization, then drying, degreasing, sintering, cooling and heat treatment step obtain medical porous tantalum material; The mass concentration of described polyvinyl alcohol water solution is 2 ~ 8%, and described vibration frequency is 20 ~ 80 beats/min; Described thermal treatment is vacuum tightness is 10
-4pa ~ 10
-3pa, is warming up to 800 ~ 900 DEG C, insulation 240 ~ 480min with 10 ~ 20 DEG C/min, then is chilled to 400 DEG C, insulation 120 ~ 300min with 2 ~ 5 DEG C/min, then cools to room temperature with the furnace.
Contriver finds in long-term R & D process, and adopting vibrations pressurization of the present invention to effectively prevent tantalum powder, to add in cavernous body the dispersiveness easily occurred bad, makes its skewness thus has a strong impact on the problem of the mechanical property of final porous tantalum material.In the R&D process of medical porous metallic substance, the material of medical porous metallic substance load bone tissue as an alternative, require its porosity comparatively large, like this tissue just easily grow into, good biocompatibility thus play its effect fully, but porosity is larger, aperture is larger, mechanical property such as intensity, toughness just can not be guaranteed; Otherwise mechanical property is got well and is easily made that porosity is too small, biocompatibility is bad, density is also excessive causes discomfort; The syntheti c route of medical porous tantalum is numerous, but contriver creatively proposes and adopts above-mentioned steps, technique prepares medical porous tantalum embedded material, the above-mentioned thermal treatment process particularly adopted, substantially eliminate internal stress, make porous tantalum materials microstructure evenly, substantially increase obtained porous tantalum material toughness and technique is quick and easy; Its obtained porous tantalum material through its foreign matter content of test can lower than 0.2%, its biocompatibility and biological safety good, density can reach 5.00 ~ 8.33g/cm
3, porosity can reach 50 ~ 70%, and pore diameter can reach 150 ~ 500 μm; Young's modulus can reach 4.5 ~ 6.0Gpa, unit elongation reaches 10.0 ~ 11.7%, flexural strength can reach 90 ~ 110Mpa, ultimate compression strength can reach 70 ~ 80Mpa, its biocompatibility, obdurability are close to the characteristic of human bearing's osseous tissue, and the porous tantalum that the present invention obtains is suitable for the medical embedded material of alternative load bone tissue very much.Meanwhile, described preparation method's technique simply, is easily controlled; Whole preparation process is harmless, pollution-free, toxicological harmless dust, has no side effect, be suitable for commercial scale production to human body.Moreover, preferentially adopt in preparation process and can all decompose in sintering process, there is no residual reagent and Organic Foam Material etc., will the biocompatibility and the biological safety that ensure embedded material be conducive to.
Further feature of the present invention is: adopt its median size to be less than 43 μm, the oxygen level ta powder that is less than 0.1%, adopting polyvinyl alcohol water solution to be binding agent and water is that dispersion agent and described tantalum powder make tantalum powder slurry, Organic Foam Material is polyurethane foam, and then vacuum-drying is except anhydrating.
Wherein, polyvinyl alcohol distilled water is heated to dissolve, adopt mass percent concentration be 4 ~ 5% polyvinyl alcohol water solution and ta powder make tantalum powder slurry, wherein, be that to add weight be in the described polyvinyl alcohol water solution of 1 part for the ta powder of 6 ~ 9 parts (preferably 7 parts) by weight, stir and make starchiness; And to adopt vibrations pressurization (vibration frequency be preferably 60 times/min, pressure be preferably 0.1MPa) to note in aperture be 0.48 ~ 0.89mm, density 0.015g/cm
3~ 0.035g/cm
3, hardness is greater than 50 °, and (preferred aperture is 0.56 ~ 0.72mm, density 0.025g/cm
3, hardness 50 ° ~ 80 °) polyurethane foam in.
Further preferably, after Organic Foam Material is injected in above-mentioned tantalum powder slurry vibrations pressurization, also uniformly spraying above-mentioned polyvinyl alcohol water solution, the weight part ratio of quantity for spray and above-mentioned ta powder is 1:6.
Prioritizing selection median size is less than 43 μm, the oxygen level ta powder that is less than 0.1% contributes to reducing the content of impurity, ensures that material has good mechanical property; Selection aperture is 0.48 ~ 0.89mm, density 0.025g/cm
3~ 0.035g/cm
3, the polyurethane foam that hardness is greater than 50 ° contributes to the porosity and the pore diameter that ensure porous tantalum.
The present invention's further feature is on the other hand: dry vacuum tightness keeps 10
-2~ 1Pa vacuum tightness, then under protective atmosphere, such as vacuum tightness 10
-4~ 10
-3pa, carries out the skimming treatment removing polyvinyl alcohol and Organic Foam Material under temperature 400 DEG C ~ 800 DEG C conditions; 10 are not less than again in vacuum tightness
-4~ 10
-3pa, temperature 2000 ~ 2200 DEG C, the soaking time vacuum sintering process of 1 ~ 5 hour obtains porous sintered body.Filling with inert gas protection vacuum protection can be replaced during sintering process insulation; Finally carry out above-mentioned vacuum annealing process.
Above-mentioned skimming treatment condition also includes: be progressively warming up to 400 ~ 800 DEG C with the speed of 0.5 DEG C/min ~ 5 DEG C/min, pass into formed protective atmosphere and be incubated 30min ~ 120min with argon gas;
Vacuum sintering condition also includes: vacuum tightness is not less than 10
-3pa, rises to 1200 DEG C ~ 1500 DEG C with the temperature rise rate not higher than 10 ~ 20 DEG C/min from room temperature, after insulation 1h ~ 2h; Again to be warming up to 2000 ~ 2200 DEG C lower than the temperature rise rate of 20 DEG C/min, be at least incubated 2h ~ 4h;
Cooling conditions after vacuum sintering also includes: vacuum tightness is not less than 10
-3pa, with not higher than 25 DEG C/min, is not less than 10 DEG C/min and gradually falls rate of cooling mode, and to sintered porous bodies segmentation cooling down to 800 DEG C, each section of soaking time 30min ~ 90min, then cools to normal temperature with the furnace;
Vacuum annealing condition also includes: vacuum tightness is 10
-4pa ~ 10
-3pa, is warming up to 800 ~ 900 DEG C, insulation 260 ~ 320min with 15 DEG C/min, then is chilled to 400 DEG C, insulation 120 ~ 300min with 3 DEG C/min, is then cooled to room temperature with 18 ~ 23 DEG C/min.
Further feature is on this basis: described vacuum drying vacuum tightness is 10
-2~ 1Pa, drying temperature 60 ~ 100 DEG C, 4 ~ 8 hours time of drying; Described skimming treatment condition also includes: be progressively warming up to 600 ~ 800 DEG C; formation protective atmosphere is passed into pure argon gas (99.9999%); 400 DEG C are risen to from room temperature with the speed of 1 ~ 5 DEG C/min; insulation 30 ~ 60min; rise to 600 ~ 800 DEG C with the speed of 0.5 ~ 1.5 DEG C/min from 400 DEG C, insulation 60 ~ 120min, described vacuum sintering condition also includes: rise to 1200 ~ 1250 DEG C with the speed of 10 ~ 15 DEG C/min from room temperature; insulation 30 ~ 60min, vacuum tightness is 10
-4pa ~ 10
-3pa; Rise to 1500 DEG C with the speed of 10 ~ 20 DEG C/min, insulation 30 ~ 60min, vacuum tightness is 10
-4pa ~ 10
-3pa, rises to 2000 ~ 2200 DEG C with the speed of 6 ~ 20 DEG C/min, and insulation 120 ~ 240min, vacuum tightness is 10
-4pa ~ 10
-3pa; Cooling conditions after vacuum sintering also includes: vacuum tightness is 10
-4pa ~ 10
-3pa; 1500 ~ 1600 DEG C are cooled to, insulation 30 ~ 60min with the speed of 10 ~ 20 DEG C/min; 1200 ~ 1250 DEG C are cooled to, insulation 60 ~ 90min with the speed of 12 ~ 20 DEG C/min; 800 DEG C are cooled to, then furnace cooling with the speed of 10 ~ 20 DEG C/min; Described vacuum annealing is: vacuum tightness is 10
-4pa ~ 10
-3pa, is warming up to 800 ~ 900 DEG C, insulation 260 ~ 320min with 15 DEG C/min, then is chilled to 400 DEG C, insulation 120 ~ 300min with 3 DEG C/min, is then cooled to room temperature with 18 ~ 23 DEG C/min.
Be wherein the content contributing to reducing impurity in porous tantalum to vacuum-drying, skimming treatment etc., improve biocompatibility and biological safety is good and mechanical property; To the optimization of Organic Foam Material material to solve the problem of not easily subsiding of foam framework in sintering process; To sintering and the optimization of process conditions of annealing steps, to improve the mechanical property of porous tantalum further as ductility etc.
Embodiment
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is that 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 according to the invention described above content to the present invention.
Embodiment 1: weighing polyvinyl alcohol 12.2g, puts into the container that 240ml distilled water is housed; Placing it in, electric furnace heats and stir makes it to become polyvinyl alcohol water solution.Weigh median size with 200g balance and be less than 43 microns, the oxygen level tantalum powder 60g that is less than 0.1%, add the polyvinyl alcohol water solution of 50ml cooling, be uniformly mixed, make it to become tantalum powder slurry.(mean pore size is 0.48mm, density 0.025g/cm to select 10 × 10 × 30mm cellular polyurethane foam
3, hardness 50 °), 55 times/min, 0.1Mpa under shake pressurization described tantalum powder slurry be poured into wherein.Dry in vacuum drying oven, drying temperature 60 DEG C, 8 hours time of drying, vacuum tightness keeps 1Pa.Skimming treatment: low vacuum is in 10
-4pa, temperature 600 DEG C, soaking time 120 minutes.Vacuum sintering: sinter in a vacuum furnace, sintering temperature 2000 DEG C, is incubated 2 hours, vacuum tightness 10
-4pa, sintering process applying argon gas is protected, and takes out after product and removes surface dirt and dirt, and obtained sample carries out cooling again, thermal treatment, and described thermal treatment is 10 in vacuum tightness
-4pa ~ 10
-3pa, is warming up to 800 ~ 900 DEG C, insulation 270min with 12 DEG C/min, then is chilled to 400 DEG C, insulation 170min with 4 DEG C/min, then cools to room temperature with the furnace, 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 lower than 0.5% finished product, its even pore distribution and be communicated with, density 6.7g/cm
3, porosity 66%, pore mean diameters 405 μm, Young's modulus 4.8GPa, flexural strength 95MPa, ultimate compression strength 72Mpa, unit elongation 10.8%.
Embodiment 2: weighing polyvinyl alcohol 10g, puts into the container that 200ml distilled water is housed; Placing it in, electric furnace heats and stir makes it to become polyvinyl alcohol water solution.Weigh median size with 200g balance and be less than 43 microns, the oxygen level tantalum powder 40g that is less than 0.1%, add 32ml polyvinyl alcohol water solution, be uniformly mixed, make it to become tantalum powder slurry.(mean pore size is 0.56mm, density 0.030g/cm to select 10 × 10 × 25mm cellular polyurethane foam
3, hardness 60 °), 60 times/min, 0.08Mpa under shake pressurization described tantalum powder slurry be poured into wherein.Dry in vacuum drying oven, drying temperature 100 DEG C, 4 hours time of drying, vacuum tightness keeps 10
-2pa.Skimming treatment: vacuum tightness 10
-4pa, temperature 800 DEG C, soaking time 120 minutes.Vacuum sintering: sinter in a vacuum furnace, sintering temperature 2100 DEG C, is incubated 4 hours, vacuum tightness 10
-4pa, sintering process applying argon gas is protected, and takes out after product and removes surface dirt and dirt, and obtained sample carries out cooling again, thermal treatment, and described thermal treatment is 10 in vacuum tightness
-3pa, is warming up to 800 ~ 900 DEG C, insulation 320min with 15 DEG C/min, then is chilled to 400 DEG C, insulation 300min with 3 DEG C/min, is then cooled to room temperature with 19 DEG C/min, 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 lower than 0.5% finished product, its even pore distribution and be communicated with, density 5.05g/cm
3, porosity 58%, pore mean diameters 330 μm, Young's modulus 6.0GPa, flexural strength 93MPa, ultimate compression strength 74Mpa, unit elongation 11.5%.
Embodiment 3: weighing polyvinyl alcohol 11g, puts into the container that 220ml distilled water is housed; Placing it in, electric furnace heats and stir makes it to become polyvinyl alcohol water solution.Weigh median size with 200g balance and be less than 43 microns, the oxygen level tantalum powder 45g that is less than 0.1%, add 36ml polyvinyl alcohol water solution, be uniformly mixed, make it to become tantalum powder slurry.(mean pore size is 0.70mm, density 0.035g/cm to select 8 × 8 × 25mm cellular polyurethane foam
3, hardness 70 °), 80 times/min, 0.2Mpa under shake pressurization described tantalum powder slurry be poured into wherein.Dry in vacuum drying oven, drying temperature 80 DEG C, 6 hours time of drying, vacuum tightness keeps 10
-1pa.Skimming treatment: vacuum tightness 10
-3pa, temperature 700 DEG C, soaking time 90 minutes.Vacuum sintering: sinter in a vacuum furnace, sintering temperature 2200 DEG C, is incubated 2.5 hours, vacuum tightness 10
-3pa, sintering process applying argon gas is protected, and cooling is come out of the stove, and removes product surface dust and dirt, and obtained sample carries out cooling again, thermal treatment, and described thermal treatment is 10 in vacuum tightness
-3pa, is warming up to 800 ~ 900 DEG C, insulation 250min with 17 DEG C/min, then is chilled to 400 DEG C, insulation 122min with 6 DEG C/min, is then cooled to room temperature with 18 DEG C/min, 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 lower than 0.5% finished product, its even pore distribution and be communicated with, density 7.5g/cm
3, porosity 55%, pore mean diameters 130 μm, Young's modulus 5.2GPa, flexural strength 106MPa, ultimate compression strength 72Mpa, unit elongation 10.4%.
Embodiment 4: weighing polyvinyl alcohol 12g, puts into the container that 230ml distilled water is housed; Placing it in, electric furnace heats and stir makes it to become polyvinyl alcohol water solution.Weigh median size with 200g balance and be less than 43 microns, the oxygen level tantalum powder 50g that is less than 0.1%, add 40ml polyvinyl alcohol water solution, be uniformly mixed, make it to become tantalum powder slurry.(aperture is 0.60mm, density 0.027g/cm to select 12 × 12 × 30mm cellular polyurethane foam
3, hardness 80 °), 23 times/min, 0.1Mpa under shake pressurization described tantalum powder slurry be poured into wherein.Dry in vacuum drying oven, drying temperature 90 DEG C, 5 hours time of drying, vacuum tightness keeps 1Pa.Skimming treatment: vacuum tightness 10
-4~ 10
-3pa, temperature 500 DEG C, soaking time 120 minutes.Vacuum sintering: sinter in a vacuum furnace, sintering temperature 2150 DEG C, is incubated 2 hours, vacuum tightness 10
-4pa, sintering process applying argon gas is protected, and cooling is come out of the stove, and removes product surface dust and dirt, and obtained sample 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 lower than 0.5% finished product, its even pore distribution and be communicated with, density 8.33g/cm
3, porosity 60%, pore mean diameters 200 μm, Young's modulus 5.0GPa, flexural strength 99MPa, ultimate compression strength 72Mpa, unit elongation 11.0%.
Embodiment 5: a kind of porous tantalum, it is less than 43 μm with particle diameter, oxygen level is less than the ta powder of 0.1% for raw material, be that binder solution makes tantalum powder slurry with polyvinyl alcohol water solution, and vibrations add pressure injection in polyurethane foam carrier, then at the above-mentioned polyvinyl alcohol water solution of surface spraying; Carry out vacuum-drying, skimming treatment, vacuum sintering, vacuum annealing and conventional aftertreatment more obtained.
Wherein, the polyurethane foam selected, its aperture is 0.72 ~ 0.56mm, density 0.025g/cm
3, hardness 50 ° ~ 80 °; Vibrations pressurization: frequency 23 times/min, 0.1Mpa;
Vacuum-drying: vacuum tightness keeps 10
-2~ 1Pa, to remove the moisture in the polyurethane foam filling tantalum powder slurry;
Skimming treatment: under protection of inert gas atmosphere or vacuum tightness 10
-4~ 10
-3pa, temperature 400 DEG C ~ 800 DEG C, and soaking time 30 ~ 120 minutes is with removing polyvinyl alcohol wherein and polyurethane foam;
Vacuum sintering: low vacuum is in 10
-4pa ~ 10
-3pa, temperature 2000 ~ 2200 DEG C, soaking time 1 ~ 5 hour, applying argon gas or other protection of inert gas during sintering process insulation, to obtain porous material;
Vacuum annealing: continue to keep temperature to be in 1000 ~ 1250 DEG C, soaking time 1 ~ 4 hour after vacuum sintering, vacuum tightness is 10
-4~ 10
-3pa, to carry out stress relief annealing process; Obtained sample 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 lower than 0.5% finished product, its even pore distribution and be communicated with, density 6.3g/cm
3, porosity 65%, pore mean diameters 290 μm, Young's modulus 4.9GPa, flexural strength 92MPa, ultimate compression strength 79Mpa, unit elongation 11.6%.
In the method that above-described embodiment 5 provides, we can also do other selections to wherein each kind of condition can obtain porous tantalum of the present invention equally.
Gained porous tantalum finished product is pressed preceding method and is detected:
| Embodiment | 6 | 7 | 8 | 9 |
| Density (g/cm 3) | 6.4 | 7.3 | 8.0 | 5.8 |
| Porosity (%) | 52 | 70 | 64 | 59 |
| Aperture (μm) | 150 | 456 | 389 | 290 |
| Young's modulus (GPa) | 4.6 | 6.0 | 5.4 | 5.0 |
| Flexural strength (MPa) | 110 | 100 | 90 | 80 |
| Ultimate compression strength (MPa) | 80 | 76 | 70 | 73 |
| Unit elongation (%) | 10.0 | 11.5 | 10.6 | 11.0 |
Claims (1)
1. prepare the method for medical porous tantalum embedded material for one kind, it is characterized in that: be less than 40 μm with particle diameter, oxygen level is less than the ta powder of 0.1% for raw material, be that binder solution makes tantalum powder slurry with polyvinyl alcohol water solution, polyvinyl alcohol water solution mass concentration 8%, tantalum powder: the weight part ratio of polyvinyl alcohol water solution is 7.5:1, and vibrations add pressure injection in polyurethane foam carrier, be then 5.5:1 at the polyvinyl alcohol water solution weight part ratio of the above-mentioned polyvinyl alcohol water solution of surface spraying, tantalum powder and polyurethane foam surface spraying; Carry out vacuum-drying, skimming treatment, vacuum sintering, vacuum annealing and conventional aftertreatment again;
Wherein, the polyurethane foam selected, its aperture is 0.68mm, density 0.035g/cm
3, hardness 55
0;
Vibrations pressurization: frequency 23 times/min, 0.1Mpa;
Vacuum-drying: vacuum tightness keeps 1Pa, the moisture that dry 6.5 hours fill in the polyurethane foam of tantalum powder slurry with removing at 65 DEG C;
Skimming treatment: under protection of inert gas atmosphere or vacuum tightness 10
-4~ 10
-3the speed of Pa, 1.5 DEG C/min rises to 400 DEG C from room temperature, insulation 58min; The speed of 0.6 DEG C/min rises to 650 DEG C from 400 DEG C, and insulation 110min is with removing polyvinyl alcohol wherein and polyurethane foam;
Vacuum sintering: the speed of 11 DEG C/min rises to 1210 DEG C from room temperature, insulation 58min, vacuum tightness is 10
-4pa; 1270 DEG C are risen to, insulation 55min with the speed of 12 DEG C/min; Rise to 2050 DEG C with the speed of 8 DEG C/min, insulation 220min, vacuum tightness is 10
-3pa; Vacuum tightness is 10
-4pa ~ 10
-3pa, is cooled to 1530 DEG C with the speed of 12 DEG C/min, insulation 55min; 1210 DEG C are cooled to, insulation 85min with the speed of 14 DEG C/min; 800 DEG C are cooled to, then furnace cooling with the speed of 14 DEG C/min;
Vacuum annealing: vacuum tightness is 10
-4pa, is warming up to 800 ~ 900 DEG C, insulation 430min with 18 DEG C/min, then is chilled to 400 DEG C, insulation 268min with 5 DEG C/min, then cools to room temperature with the furnace, to carry out stress relief annealing process; Obtained sample carries out conventional aftertreatment again and obtains porous tantalum finished product.
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| EP3326662A4 (en) * | 2015-09-21 | 2019-04-03 | Chongqing Runze Pharmaceutical Co. Ltd. | Use of porous material |
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| CN110468401A (en) * | 2018-05-11 | 2019-11-19 | 中国科学院金属研究所 | A kind of method that cold spraying prepares porous tantalum bioactivity coatings |
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| EP3326662A4 (en) * | 2015-09-21 | 2019-04-03 | Chongqing Runze Pharmaceutical Co. Ltd. | Use of porous material |
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| CN103740967A (en) | 2014-04-23 |
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