CN1850292A - Method for making foam biological titanium alloy artificial skelecton with hollow structure - Google Patents
Method for making foam biological titanium alloy artificial skelecton with hollow structure Download PDFInfo
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- CN1850292A CN1850292A CN 200610026678 CN200610026678A CN1850292A CN 1850292 A CN1850292 A CN 1850292A CN 200610026678 CN200610026678 CN 200610026678 CN 200610026678 A CN200610026678 A CN 200610026678A CN 1850292 A CN1850292 A CN 1850292A
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Abstract
The present invention relates to an once-formed production method of foamed biological titanium alloy artificial bone with hollow structure. Said method includes the following steps: adding one of Na, Ta, Mo, W, Zr, Hf, Y, La, Tc, Ru, Rh, Re, Os and Ir or their combination in titanium alloy, adding one of Cu-Ni-Zr, Cu-Ni-Sn, Co-Cu-Sn and Cu-Ni-Sn-Si-B, then preparing casting mould with bone-shaped hollow cavity, melting alloy in the vacuum environment, and pouring the molten alloy into the casting mould with bone-shaped hollow cavity.
Description
Technical field
The present invention relates to a kind of method of technical field of bioengineering, specifically is a kind of method for making foam biological titanium alloy artificial skelecton with hollow structure.
Technical background
In the metallic biomaterial, the cobalt chromium of the rustless steel of the first generation and the second filial generation or vitallium are because its elastic modelling quantity, is unfavorable for reproducing and healing of natural skeleton tissue more than the skeleton height after the implantation, so clinical practice is gradually reducing.Biological titanium alloy is compared with the first and second substituting metal biomaterials has obvious superiority, for example, very ideal bio-compatibility, outstanding corrosion resistance, high fatigue strength, low elastic modulus, so titanium alloy is that long-acting or permanent human body is implanted optimal metallic biomaterial.
Though the elastic modelling quantity of biological titanium alloy far below the first and second substituting metal biomaterials, is compared still too high (biological titanium alloy: 50～120GPa with natural skeleton; Bone: 20～30GPa), wherein an approach of Xie Jueing is preparation titanium foam or a titanium foam alloy, to obtain low elastic modulus, metallic biomaterial that intensity is moderate.On the other hand, foam metal material not only elastic modelling quantity and natural skeleton mates more, and wherein the foam hole of Cun Zaiing also has great significance to the healing that promotes tissue.If further in the artificial skelecton of foaming structure, produce the cavity, center, then the hole of Guan Tonging can provide that bone marrow or body fluid exist, mobile space, help effective connection the between implant and natural skeleton, activate osteocyte around implant and the normal growth of inner pore, further improve the recovery of ill organ after implanting or limb function.
Find through literature search prior art, the foam artificial skelecton manufacturing technology that does not have hollow structure, has only traditional foam metal manufacturing technology, making principle according to it can be divided three classes traditional process for preparing foam metal: (1) powder metallurgy process is made foam metal, through process procedures such as metal powder process, compression moulding, sintering, advantage is that vesicular tissue is even, porosity is regulated easily, and shortcoming is complex process, cost height.C.E.Wen " Processing of biocompatible porous Ti and Mg " (titanium foam of bio-compatible and the foam magnesium manufacture process) on " Scripta Materialia " (material periodical) calendar year 2001 the 45th volume 1147-1153 page or leaf, delivered for example, adopt powder metallurgy process to make titanium foam and magnesium in this article, concrete grammar is: at first prepare titanium or magnesium dust, base, compacting then, sintering in the vacuum again, its deficiency is: technical process is very complicated, multiple working procedure, the manufacturing cost height.(2) liquid metal and gas physical mixed method are made foam metal, by injecting gas in liquid metal, the cooling back forms foam metal, advantage is that technology is simple, shortcoming is that stomatal frequency and uniformity are not easy accurate control, also should avoid reacting with metal for the gas that injects liquid metal.For example A.E.Simone rolled up " Aluminumfoams produced by liquid-state processes " (the producing foamed aluminium by liquid process) of delivering on the 3109-3123 page or leaf in 1998 the 46th at " ActaMaterialia " (material periodical), adopt in this article and in liquid aluminium, blow, cool off liquid aluminium then, make it solidify the formation foamed aluminium, its deficiency is technical process control difficulty, foaming structure is inhomogeneous, and is not suitable for the preparation of the higher alloy foam material of liquid viscosity.(3) solid-gas phase eutectic freezing method, there are eutectic reaction in metal and gas phase that this method requires to solidify, therefore have significant limitation.
Though adopt the foam metal of traditional method manufacturing to be used to make artificial skelecton, up to now also without any the foam metal artificial skelecton of the hollow structure of form.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of method for making foam biological titanium alloy artificial skelecton with hollow structure is provided, make its manufacturing have the foam biological titanium alloy artificial skelecton of hollow structure, foaming structure wherein and skeleton hollow structure all are once to form in casting process, do not need additional machining, there is good connectedness in space in its center cavity and the foaming structure, the infiltration that helps body fluid or bone marrow has improved the biological characteristics of artificial skelecton greatly with mobile.
The present invention is achieved by the following technical solutions, the present invention at first designs and can cast out the titanium alloy component with hollow structure, titanium alloy with design, by the composition proportion combination, heat fused in vacuum system, cast in then in the mold of skeletal shape, by the mold natural cooling, make liquid alloy solidify to form the solidified structure of foaming structure and at bone shape sample central shaft to forming the cavity, thereby in the one-step casting process of setting, obtain to have the foam biological titanium alloy artificial skelecton of hollow structure.
The present invention specifically comprises following step:
1. form the composition design of the titanium foam alloy of hollow: two stages of structure alloy (initial+eutectic) consecutive solidification, the temperature difference of two stages of alloy of design between solidifying is at 500 to 2500 degree, utilize the cooling of initial solidification and eutectic freezing alloy liquid phase between two stages to shrink, form the vesicular tissue and the hollow structure of bone shape foundry goods.Concrete method is, by add refractory metal or stable beta phase metal in titanium alloy, for example: Nb, Ta, Mo, W, Zr, Hf, Y, La, Tc, Ru, Rh, Re, Os, Ir one of them or wherein two combinations make alloy can at first solidify in the liquid phase cools process and separate out dystectic beta-Ti solid solution, and form three-dimensional netted dendritic structure; By adding low-melting relatively metal or nonmetal combination, for example: Cu-Ni-Zr, Cu-Ni-Sn, Co-Cu-Sn, Cu-Ni-Sn-Si-B or the like, make the raffinate phase constituent behind the alloy generation initial solidification have low melting point, so that be distributed in residue liquid phase in the three-dimensional netted dendritic structure before eutectic freezing takes place, experience big cooling, shrink thereby produce big cooling, form the cavity, be dispersed in the voidage of the cavity formation titanium foam alloy in the three-dimensional netted dendritic structure.Further, finally in bone shape foundry goods, be formed centrally the cavity, have the purpose of hollow structure foam titanium alloy artificial skelecton thereby reach to make because the radial symmetry gradient that bone shape die cavity forms causes consecutive solidification from outside to inside.
Summarize alloy designs thinking described above and method, can will form the following formal representation of titanium foam alloying component of hollow:
(Ti
aM
b)
x(Ti
cE1
dE2
eE3
f)
1-x
(Ti wherein
aM
b) expression forms the one-tenth subdivision of high-melting-point beta-Ti solid solution, M represents that the metal of refractory metal or stable beta phase: M can be Nb, Ta, Mo, W, Zr, Hf, Y, La, Tc, Ru, Rh, Re, Os, Ir one of them or wherein both combinations.(Ti
cE1
dE2
eE3
f) expression forms the metal or the nonmetal assembled unit of low melting point eutectic composition, wherein: E1 can be V, Cr, Mn, Fe, Co, Ni, Cu, Pd, Ag, Pt, Au one of them; E2 can be Al, Zn, Ga, Cd, In, Sn, Sb, Hg, Tl, Pb, Bi, Po one of them; E3 can be Si, B, C, Be, Li, Sc, Mg one of them.Parameter area in the following formula (atomic percentage), wherein, a=100-b, b=5-50; C=100-(d+e+f), d=0-20, e=0-20, f=0-10; X=0.4-0.9 is by changing the voidage that x can regulate the titanium foam alloy.
2. select vacuum metal die cast or other vacuum precision casting method for use, the mold of preparation bone shape cavity.Different casting methods can provide solidifies the cooling condition difference, can cause the foundry goods of different voidages.Simultaneously, the related manufacturing cost of different casting methods is also different, therefore, for production application of the present invention, can select best casting method according to the requirement of voidage and the taking all factors into consideration of manufacturing cost to the artificial skelecton foaming structure.
3. with the titanium foam alloy of above design assignment system proportionately, fusing is cast in the mold with bone shape cavity then in a vacuum.In process of setting and since alloying component comprised dystectic initial solidification mutually and low-melting eutectic freezing mutually, will at first form three-dimensional netted dendritic structure, and be accompanied by temperature and reduce, the liquid phase between netted branch produces shrinks, the formation foaming structure.Because there is thermograde in foundry goods from the surface to the center, make the three-dimensional netted branch foaming structure that forms from the cast(ing) surface to the center, have consecutive solidification, the foundry goods center of final set is because no liquid feeding, to in foundry goods, be formed centrally the cavity of perforation, thereby form foam titanium alloy artificial skelecton with hollow structure.
For key point of the present invention is had further understanding, below ultimate principle of the present invention is described in greater detail, two stages that constructed when the titanium foam design of alloy are solidified (initial solidification+eutectic freezing), and the temperature difference of solidifying for twice is in the 500-2500K scope, the alloy that solidifies for the first time (initial solidification) is the beta-Ti solid solution with the bcc structure of three-dimensional tree dendritic growth, interconnect between the branch, form tridimensional network, residual metallic between branch takes place to solidify (eutectic freezing) before for the second time, produce liquid the contraction, shrink the cavity thereby between three-dimensional netted dendritic structure, form, finally form the titanium foam alloy.The form of three-dimensional netted dendritic structure and yardstick are relevant with the cooling condition of alloying component and process of setting, and generally speaking, if cooling is fast more, foaming structure is fine and closely woven more.When casting titanium foam alloy bone shape foundry goods, adopt cooling mold fast, can so that foundry goods from the surface to be formed centrally higher thermograde, the liquid metal rapid solidification of casting back contact model wall forms fine and closely woven foaming structure, past more center, rate of cooling is low more, the foaming structure that forms is thick more, and the central shaft that in the end solidifies is empty to forming, and the size in cavity, center depends on alloying component, solidifies cooling condition, the casting dimension size.
The present invention vacuum metal die cast or other casting method, the simulating nature skeletal shape casts out the foam titanium alloy artificial skelecton with hollow structure.Manufacture method of the present invention is simple, vesicular tissue evenly and easily controls, and can one-shot forming produce foam titanium alloy artificial skelecton with hollow structure, than present most foams biological titanium material all have higher mechanical property for example elastic modelling quantity more near natural skeleton; Proportion is littler; Specific strength is higher or the like.Wherein the artificial skelecton of hollow structure is to invent first, simulated the structure of natural skeleton well, it can provide, and bone marrow or body fluid exist, mobile space, make the bone marrow bone liquid in artificial skelecton, to permeate and flow, the healing and the organization restructuring that help skeleton further improve the recovery of implanting ill organ in back or limb function.
Description of drawings
Fig. 1 is the foam biological titanium alloy composition phasor principle with hollow structure
Fig. 2 is the gradient foam biological titanium alloy skeleton sketch map with hollow, and wherein: (a) Thigh bone, (b) the gradient foam titanium alloy skeleton with hollow is cast in simulation, (c) has the gradient foam titanium alloy skeleton microstructure sketch map of hollow.
Fig. 3 is the (Ti with gradient foam tissue and hollow structure
80Nb
20)
0.5(Ti
40Cu
28Ni
24Sn
8)
0.5The bar-shaped example cross section photo of alloy, wherein: (a) sample diameter 3mm, (b) sample diameter 5mm.
Fig. 4 is the (Ti with gradient foam tissue and hollow structure
80Nb
20)
0.5(Ti
40Cu
28Ni
24Sn
8)
0.5The bar-shaped example cross section photo of alloy 3mm diameter, wherein: (a) hollow and peripheral vesicular tissue, (b) vesicular tissue of Fang Daing.
Fig. 5 is the bar-shaped example cross section photo of alloy with gradient foam tissue and hollow structure, and wherein: alloying component is Ti among the figure a
48.75Zr
4.875Mo
2.5Cu
24.375Ni
14.625Sn
4.875, alloying component is Ti among the figure b
47.5Zr
4.75Mo
5Cu
23.75Ni
14.25Sn
4.75
The specific embodiment
Below in conjunction with drawings and Examples technical solution of the present invention is done further to understand:
Figure 1 shows that foam biological titanium alloy composition principle phasor with hollow structure, the foamed alloy composition is made up of two parts: (1) has dystectic beta-Ti solid solution, by in titanium alloy component, adding the refractory metal or the stable beta phase metal of certain content, as Ta, Nb, Mo, W, Zr, Hf etc., thereby guarantee when initial solidification, can form the dendritic network structure of three-dimensional tree, beta-Ti (M) is the main phase of titanium foam alloy mutually, and its form and size are the major parameters of decision foaming structure yardstick and density.(2) has low-melting eutectic composition, by adding the metal or the nonmetal combination of certain content, as Cu-Ni-Zr, Cu-Ni-Sn, Co-Cu-Sn, Cu-Ni-Sn-Si-B etc., in titanium alloy, form low-melting eutectic composition, before eutectic freezing takes place, has liquid alloy very large cooling (T of experience between dendroid beta-Ti (M) phase of eutectic composition
l-T
e=500-2500K), shrink thereby produce significant cooling, between three-dimensional branch, form the cavity, finally form the titanium foam alloy.
Figure 2 shows that gradient foam biological titanium alloy skeleton sketch map with hollow, its microstructure (Fig. 2 c) shows, is to have little voidage, the foaming structure of compact structure near cast(ing) surface, towards the foundry goods center, the foam voids rate increases, and has been formed centrally hollow structure in foundry goods.
Embodiment 1
Add Nb in the alloy and form dystectic beta-Ti solid solution, add Cu-Ni-Sn and be combined to form the low melting point eutectic composition, for example composition is (Ti
80Nb
20)
0.5(Ti
40Cu
28Ni
24Sn
8)
0.5Titanium alloy, by die cast, can form gradient foam biological titanium alloy skeleton with hollow.Figure 3 shows that the bar-shaped example cross section photo of foamed alloy, (a) 3mm diameter sample, (b) 5mm diameter sample.Sample diameter difference, cooldown rate are then different, so hollow diameters varies in size, and increase with sample diameter, and hollow diameters increases.Figure 4 shows that the bar-shaped example cross section of 3mm diameter vesicular tissue photo, (a) hollow and peripheral vesicular tissue, (b) vesicular tissue of Fang Daing, the visible reticulated polymer foam tissue that constitutes by dendrite relatively uniformly in the photo (a), after further amplifying, as seen white beta-Ti dendrite is surrounded by the Lycoperdon polymorphum Vitt eutectic phase, and the black cavity that distributes between branch.(Ti in the present embodiment
80Nb
20) (the Ti of corresponding (1) formula
aM
b), its effect is to form dystectic netted dendrite, as the white phase among Fig. 4 b, (Ti
40Cu
28Ni
24Sn
8) (the Ti of corresponding (1) formula
cE1
dE2
eE3
f), be the main component that forms low melting point eutectic, in alloy, play the effect that cooling is shunk, formed space between the netted dendrite.This composition has satisfied the titanium foam design of alloy scope that the present invention relates to, and has adopted after the vacuum metal die cast, has obtained to have the titanium foam alloy skeleton shape foundry goods of hollow structure, as shown in Figure 3 and Figure 4.
Embodiment 2
Add different beta-Ti solid solution forming elements in the alloy, can obtain the three-dimensional dendritic structure of different shape and different hollow structures.As add Zr and Mo forms dystectic beta-Ti solid solution, and add Cu-Ni-Sn and be combined to form the low melting point eutectic composition, for example composition is Ti
48.75Zr
4.875Mo
2.5Cu
24.375Ni
14.625Sn
4.875Titanium alloy, by the vacuum metal die cast, can form gradient foam biological titanium alloy skeleton with hollow.Fig. 5 a is depicted as the bar-shaped example cross section photo of foamed alloy, the vesicular tissue around the black at show sample center cavity and the cavity of maying be seen indistinctly clearly in the photo.This composition has satisfied the titanium foam design of alloy scope that the present invention relates to, and has adopted after the vacuum metal die cast, has obtained to have the titanium foam alloy-steel casting of hollow structure.
Embodiment 3
By changing the relative composition of alloy among the embodiment 2, as increasing beta-Ti solid solution forming element Mo, reduce the alloying element that forms the low melting point eutectic composition, can obtain the foundry goods of different hollow structures.For example composition is Ti
47.5Zr
4.75Mo
5Cu
23.75Ni
14.25Sn
4.75Titanium alloy, by the vacuum metal die cast, can form gradient foam biological titanium alloy skeleton with hollow.Fig. 5 b is depicted as the bar-shaped example cross section photo of foamed alloy, the vesicular tissue around the black at show sample center cavity and the cavity of maying be seen indistinctly clearly in the photo.This composition has satisfied the titanium foam design of alloy scope that the present invention relates to, and has adopted after the vacuum metal die cast, has obtained to have the titanium foam alloy-steel casting of hollow structure.
Claims (2)
1, a kind of method for making foam biological titanium alloy artificial skelecton with hollow structure is characterized in that, comprises following three steps:
1. form the composition design of the titanium foam alloy of hollow: two stage consecutive solidifications of structure alloy, the temperature difference of two stages of alloy of design between solidifying be at 500 to 2500 degree, utilize initial solidification and eutectic freezing between two stages the cooling of alloy liquid phase shrink, form the vesicular tissue and the hollow structure of bone shape foundry goods, concrete method is: by add Nb in titanium alloy, Ta, Mo, W, Zr, Hf, Y, La, Tc, Ru, Rh, Re, Os, Ir one of them or wherein two combinations make alloy at first solidify in the liquid phase cools process and separate out dystectic beta-Ti solid solution, and form three-dimensional netted dendritic structure; By adding Cu-Ni-Zr, Cu-Ni-Sn, Co-Cu-Sn, one of among the Cu-Ni-Sn-Si-B, make the raffinate phase constituent behind the alloy generation initial solidification have low melting point, be distributed in residue liquid phase in the three-dimensional netted dendritic structure before eutectic freezing takes place, experience big cooling, thereby producing big cooling shrinks, form the cavity, be dispersed in the voidage of the cavity formation titanium foam alloy in the three-dimensional netted dendritic structure, simultaneously because the radial symmetry gradient that bone shape die cavity forms, cause consecutive solidification from outside to inside, finally in bone shape foundry goods, be formed centrally the cavity;
2. use vacuum metal die cast or vacuum precision casting method, the mold of preparation bone shape cavity;
3. with the titanium foam alloy of above design assignment system proportionately, fusing is cast in the mold with bone shape cavity then in a vacuum.
2, the method for making foam biological titanium alloy artificial skelecton with hollow structure according to claim 1 is characterized in that, forms the following formal representation of titanium foam alloying component of hollow:
(Ti
aM
b)
x(Ti
cE1
dE2
eE3
f)
1-x
(Ti wherein
aM
b) expression forms the one-tenth subdivision of high-melting-point beta-Ti solid solution, M represents the metal of refractory metal or stable beta phase, M is Nb, Ta, Mo, W, Zr, Hf, Y, La, Tc, Ru, Rh, Re, Os, Ir one of them or wherein both combinations;
A and b represent atomic percentage in the formula, wherein: a=100-b, b=5-50;
(Ti in the formula
cE1
dE2
eE3
f) expression forms the metal or the nonmetal assembled unit of low melting point eutectic composition, wherein: E1 is V, Cr, Mn, Fe, Co, Ni, Cu, Pd, Ag, Pt, Au one of them; E2 is Al, Zn, Ga, Cd, In, Sn, Sb, Hg, Tl, Pb, Bi, Po one of them; E3 is Si, B, C, Be, Li, Sc, Mg one of them;
C in the formula, d, e and f represent atomic percentage, wherein: c=100-(d+e+f), d=0-20, e=0-20, f=0-10;
X represents atomic percentage in the formula: x=0.4-0.9, and by changing the voidage that x regulates the titanium foam alloy.
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|---|---|---|---|
| CNB2006100266782A CN100544776C (en) | 2006-05-18 | 2006-05-18 | Method for making foam biological titanium alloy artificial skelecton with hollow structure |
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| CN100544776C CN100544776C (en) | 2009-09-30 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372201A (en) * | 2014-11-04 | 2015-02-25 | 无锡贺邦金属制品有限公司 | Alloy material for heart stents with antiallergic function |
| CN106267333A (en) * | 2014-11-07 | 2017-01-04 | 吴昊 | A kind of antibacterial ability and the preferable biomedical metallic material of decay resistance |
-
2006
- 2006-05-18 CN CNB2006100266782A patent/CN100544776C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372201A (en) * | 2014-11-04 | 2015-02-25 | 无锡贺邦金属制品有限公司 | Alloy material for heart stents with antiallergic function |
| CN106267333A (en) * | 2014-11-07 | 2017-01-04 | 吴昊 | A kind of antibacterial ability and the preferable biomedical metallic material of decay resistance |
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| Publication number | Publication date |
|---|---|
| CN100544776C (en) | 2009-09-30 |
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