CN101660076A - Macro mesh structural porous tantalum prepared by dipping and sintering organic foams - Google Patents
Macro mesh structural porous tantalum prepared by dipping and sintering organic foams Download PDFInfo
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- CN101660076A CN101660076A CN200910204811A CN200910204811A CN101660076A CN 101660076 A CN101660076 A CN 101660076A CN 200910204811 A CN200910204811 A CN 200910204811A CN 200910204811 A CN200910204811 A CN 200910204811A CN 101660076 A CN101660076 A CN 101660076A
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Abstract
The invention relates to a macro mesh structural foamed porous tantalum material. The pores of the materials are classified into two kinds: main pores; and small pores and micropores. The main pores form the macro mesh structure and have the sizes between 0.5-2.0mm. The small pores and the micropores are arranged on the walls and edges of the main pores and have the sizes respectively less than and much less than the sizes of the main pores. The main pores have macro open-pore and semi-open-pore structures, the two kinds of pores are mutually communicated, and the porosity is higher than 70%.The preparation method of the high-porosity porous tantalum comprises the steps of taking the organic foams as the matrices and employing dipping, drying and sintering processes to prepare the poroustantalum. The sintering temperature ranges from 1600 DEG C to 1800 DEG C. Slurry is composed of tantalum powder and nontoxic organic binders, and the viscosity is regulated by deionized water.
Description
Technical field:
The present invention relates to the porous tantalum material, relate in particular to the preparation method of the mesh structural porous tantalum of a kind of macroscopical class.
Background technology:
Tantalum is VB family the 6th period element, and ordination number is 73, and relative atomic mass is 180.95, and volume density is 16.6g/cm
3, fusing point is only second to tungsten and rhenium near 3000 ℃ (2980 ± 20 ℃), belong to rare refractory metal ([1] Xia Fengjin, Liu Peisheng, Zhou Maoqi. the preparation method of porous tantalum [J]. the scientific and technical innovation Leader, 2008,1:83-85.).The tantalum quality is hard, and hardness can reach HV120, has good ductility simultaneously.Its thermal expansivity is very little, and every rising only expands about 6/1000000ths. six for one degree centigrade.In addition, tantalum also has characteristics such as high erosion resistance, wear resistance and excellent biological compatibility.More than these characteristics make metal tantalum obtain to use widely in fields such as chemical industry, metallurgy, electronics, electric, medical science, can be used for aspect ([1] Xia Fengjin such as chemical reaction equipment, vacuum oven, electrical condenser, nuclear reactor, aerospacecraft, guided missile and surgery embedded material, Liu Peisheng, Zhou Maoqi. the preparation method of porous tantalum [J]. the scientific and technical innovation Leader, 2008,1:83-85; [2] should be bright. porous tantalum and the application [J] in joint prosthesis. biological orthopaedics material and clinical study, 2006,3 (2): 1-3.).For example, with porous tantalum as the anodic electrical condenser have the encapsulation little, capacitance is big, the life-span is long, steady performance ([3] He Jilin. tantalum niobium electronic material new development [J]. the China YouSe Acta Metallurgica Sinica, 2004,5:291-300.), and characteristics such as suitable physical strength, Young's modulus, solidity to corrosion and excellent biological compatibility, make again porous tantalum be applicable to human synovial alternative implantation ([2] should be bright. porous tantalum and application [J] in joint prosthesis. biological orthopaedics material and clinical study, 2006,3 (2): 1-3; [4] Wu Quan is emerging. metallicity biomaterial [J]. and the rare metal wall bulletin, 2002,5:17-19.).Document ([2] should be bright. porous tantalum and the application [J] in joint prosthesis. and biological orthopaedics material and clinical study, 2006,3 (2): 1-3; [5] Bobyn J D, Stackpool G J, Hacking S A, et al.Characteristics of bone ingrowth and interface mechanics of a new porous tantalumbiomaterial[J] .J Bone Joint Surg B, 1999,81 (5): 907-914; [6] Bobyn J D, Poggie R E, Krygier J J, et al.Clinicalvalidation of a structural porous tantalum biomaterial for adult reconstruction[J] .J Bone Joint Surg A, 2004,86 (S2): 123-129; [7] Welldon K J, Atkins G J, Howie D W, et al.Primary human osteoblasts grow into poroustantalum and maintain an osteoblastic phenotype[J] .Journal of Biomedical materials Research A, 2008,84 (3): 691-701; [8] Patil N, Lee K, Goodman S B.Porous Tantalum in Hip and Knee Reconstructive Surgery[J] .Journalof Biomedical Materials Research B, 2009,89 (1): 242-251.) the porous tantalum preparation method of Jie Shaoing is, elder generation's pyrolysis polyurethane foam obtains the carbon network skeleton, the mode of metal tantalum by chemical vapour deposition is covered on the carbon skeleton again, thereby obtains three-dimensional netted porous tantalum product.The present invention adopts organic foam dipping drying and sintering technology, has prepared the mesh structural porous tantalum material of macroscopical class, and it mainly is the grand hole (macroporosity that naked eyes visual) of yardstick in the millimeter magnitude that its hole is formed, and promptly grand hole constitutes the main aperture of porous insert.
Summary of the invention:
The object of the present invention is to provide spumescence porous tantalum material that a kind of porosity height, hole be interconnected and preparation method thereof.The preparation method adopts organic foam matrix soaking paste drying and sintering technology, selects high purity tantalum powder and nontoxic cakingagent preparation slip for use, and selecting polyurethane foam for use is organic matrix.
Foam state porous tantalum material of the present invention, " reprint " form of organic foam plastic to a certain extent, it is characterized in that: by organic foam matrix soaking paste drying, thermolysis organism and realize the tantalum powder sintering under vacuum environment, form porosity at last and be 70%～85% quasi-network structure porous insert, it mainly is the grand hole (macroporosity that naked eyes visual) of yardstick at 0.5～2.0mm that its hole is formed, and is interconnected between the hole.In the porous insert, on the hole rib and hole wall that with grand hole are main aperture, exist take measurements greatly less than with aperture and micropore much smaller than main aperture.
The nontoxic cakingagent that the present invention uses is by methylcellulose gum and deionized water preparation, and both quality proportionings are 1: 5～1: 15; Drying process condition after the organic matrix soaking paste provided by the invention is more than 120 ℃ of oven dry 2h in the loft drier, to guarantee to remove in the porous body most moisture content and to make the base substrate through-hardening.
Consider the high temperature oxidation of metal tantalum, this process stipulation sintering oven should vacuumize continuously so that vacuum tightness remains on 10
-2The level of Pa.
The porous tantalum structure of the present invention's preparation has following characteristics and advantage:
1) foam state porous tantalum of the present invention is macroscopical quasi-network structure, is interconnected porosity height (can be higher than 70%) between the hole.
2) foam state porous tantalum of the present invention " reprint " structural form of used organic foam matrix in the soaking paste technology to a certain extent, has just increased the hole wall of some main apertures, and has had the micropore of a large amount of connectivities on this hole wall.The manufacturing process maturation of organic foam material, adjustability are strong, Controlled Pore Structure is good, wide in variety.Therefore, when this technology was selected porous matrix for use, available property was strong, more easily obtained the standby body of desired structure index.
3) preparation method of the present invention is easy to operate, and equipment is simple, and is practical.
Description of drawings:
The low power optical photograph of Fig. 1 porous tantalum of the present invention has shown the visual netted macro morphology of class of naked eyes in the vesicular structure, is interconnected between the hole wherein.
The low power scanning electron photomicrograph of Fig. 2 porous tantalum macro morphology of the present invention, shown exist on the hole rib of porous insert main aperture and the hole wall take measurements greatly less than with aperture and micropore much smaller than main aperture.
On main aperture hole rib in Fig. 3 porous tantalum structure of the present invention and the hole wall a large amount of micropores have a form, these micropores have further ensured the connectedness of all holes in the porous insert.
Particle combination form in Fig. 4 porous tantalum structure of the present invention shows that above-mentioned micropore is to be formed by the crystal grain crane span structure that constitutes main aperture hole rib and hole wall.
Crystal grain combined in Fig. 5 porous tantalum structure of the present invention has shown the sintering and the bonding state of crystal grain in the porous insert.
Embodiment:
Embodiment: take by weighing a certain amount of methylcellulose gum, add deionized water at normal temperature in the ratio of " methylcellulose gum: deionized water at normal temperature=1g: 8ml ", it is stand-by to be mixed with starchy even emulsus cakingagent under stirring.Selecting granularity for use is the following high purity tantalum powder of 300 orders, and the above-mentioned cakingagent of 75g tantalum powder and 25ml is mixed with slip, stirs.Carry out soaking paste with urethane through-hole foam block then and handle, the porous insert of handling that will handle is placed loft drier, in 120 ℃ of oven dry 4h.Porous insert hardening after the oven dry is put in the vacuum oven again, at room temperature is evacuated to 10 earlier
-2The level of Pa, the time with 30min is warming up to 120 ℃ again, and insulation 3h continues to vacuumize that to make pressure be 10
-2The magnitude of Pa.Time with 130min rises to 1500 ℃ with furnace temperature by 120 ℃ then, then with the time of 1h furnace temperature is brought up to 1600 ℃ by 1500 ℃, at 1600 ℃ of insulation 3h, closes heater switch after finishing and makes system's furnace cooling.Whole process keeps vacuum state, is cooled to 100 ℃ until body of heater, just stops vacuum pump and the sampling of coming out of the stove.The macro morphology of gained block body stephanoporate tantalum is the visual quasi-network structure of naked eyes (referring to Fig. 1), its pore morphology of electronic microscope photos is mainly divided two classes (Fig. 2～4), one class is that the yardstick of formation porous insert macroscopic view quasi-network structure is the main aperture of 0.5～2.0mm, another kind of is to be present in to constitute the micropore that is of a size of several micron dimensions on main aperture hole wall and the hole rib, is interconnected between the hole.It is about 80% that the volume weighting method records its porosity.
Claims (4)
1. foam state porous tantalum material, it is characterized in that: this product is macroscopical quasi-network structure, porosity is higher than 70%, hole has two classes: the one, constitute macroscopical quasi-network structure and be of a size of the main aperture of 0.5～2.0mm, the 2nd, on main aperture hole wall and the hole rib size less than with aperture and micropore much smaller than main aperture.Be interconnected between the hole.
2. the described foam state porous tantalum of claim 1 preparation methods, adopt organic foam matrix soaking paste drying and sintering method, it is characterized in that: used organic foam is a urethane foam, slurry is made up of tantalum powder, methylcellulose gum and water, wherein tantalum powder degree is below 300 orders, tantalum powder purity is higher than 99%, water is regulated viscosity, dry more than the 2h through 100～120 ℃ earlier after the soaking paste of organic foam matrix, make its moisture evaporation and acquisition have the precast body of good self-supporting hard structure, place the vacuum oven sintering then.
3. preparation method according to claim 2 is characterized in that: the tantalum powder need not pre-treatment, and slip preparation water is a deionized water, and wherein the mass ratio of methylcellulose gum and deionized water is between 1: 5～1: 15.
4. preparation method according to claim 2 is characterized in that: the vacuum tightness of sintering oven remains on 10
-2The level of Pa gets final product, and heat-up rate is 5～15 ℃/min, then at 1600～1800 ℃ of insulation 2～5h, furnace cooling.
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