CN101549175A - Method for preparation of pore heterogeneous distribution bionic bone material - Google Patents
Method for preparation of pore heterogeneous distribution bionic bone material Download PDFInfo
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Abstract
The invention discloses a method for the preparation of a pore heterogeneous distribution bionic bone material. The invention takes HA/Ti or HA/316L composite powder as raw material and forms a compact layer/a transition layer/a sparse layer by separating the raw material powder within a mould, a compact is obtained by general pressing under the pressure of 100-300MPa; the compact is sintered in vacuum and is subjected to heat preservation for 1.5-2 hours at 800 DEG C, and the temperature is then heated up slowly to sintering temperature from 1050-1250 DEG C, followed by the heat preservation. The bionic bone material obtained from the invention has the compact layer as the outer layer, the porosity of the transition layer is 38-60%, the pore diameter of 100-500 [mu]m accounts for 30-70%, the porosity of the inner layer is 57-80%, the pore diameter of 100-500 [mu]m accounts for 50-80%, the pore structures are all interconnected pores and can meet the demand of the pore size of 0-500 [mu]m by a human body bone tissue Haversian system; the inventive material integrates excellent biocompatibility and dynamic performances and has extensive clinical application prospect in repairing and reconstructing on loaded bones.
Description
Technical field
The invention belongs to technical field of biological material, particularly pore heterogeneous distribution bionic bone material.
Background technology
Osseous tissue is a human body hard tissue, uses other material to substitute the pathological changes osseous tissue with the existing many decades of the research that reaches treatment and repair.It is generally acknowledged that the chemical constituent element in the material should be similar to the major components of osseous tissue, its distribution of pores also should be with the outer cortex bone densification of people's bone the loose structure of internal layer spongy bone identical, have no side effect, can guarantee that like this it has good biocompatibility and biological degradability, to promote the growth of freshman bone tissue.
Hydroxyapatite (HA) contains the inorganic constituents similar to body bone tissue, and after implanting, under the effect of body fluid, calcium and the phosphorus material surface that can dissociate is absorbed by body, and can form chemical bond with the skeleton tissue and combine the tissue that growth makes new advances.Therefore, hydroxyapatite is the biomaterial with excellent biological compatibility and bone guided (being biological activity) of generally acknowledging at present.
The human body bone is made up of fine and close cortical bone of skin and the loose spongy bone of internal layer, outer fine and close cortical bone provides main mechanics to support, and the pore structure of the loose spongy bone of internal layer is along being subjected to the different non-uniform Distribution of force direction, this structure makes it can adapt to the STRESS VARIATION of certain limit, and to applied stress generation cushioning effect, porous organization can impel blood circulation simultaneously, guarantees the homergy growth of osseous tissue.
The fine and close skin of non-homogeneous distribution of pores bionic composite material can provide mechanics to support as cortical bone, and the porous internal layer is growing into of inducting osseous tissue then.The aperture of interconnected pore allows growing into of fibrous tissue when 5~40 μ m; When the aperture is 40~100 μ m, allow the osteoid tissue of non-mineralising to grow into; The aperture can provide desirable place for growing into of osseous tissue when 150 μ m.After porous HA implants, soft or hard is organized in the hole of all growing into, be formed the cross coupled state of fibrous tissue and freshman bone tissue, this interface energy keeps normal metabolism relation, and the interfacial structure of bone-material reaches the physiological combination.When porosity surpasses after 50%, can interconnect the cambium inside of can growing into from the surface of artificial bone between the hole, and mutually combine, so not only obtained the good interface combination, and growing into of cambium both reduce the fragility of porous HA, improved intensity again.In addition,, help the conduction of interfacial stress, meet the interface mechanics requirement, make interface energy keep stable, thereby improve planting effect owing to porous has reduced the rigidity of HA material.
Along with improving constantly of medical technique level, improve constantly for the requirement of synthetic bone alternate material.Synthesize and use the compacted zone/transition zone/weaker zone composite of the non-homogeneous distribution of pores of bionical human body bone, caused scientist and clinician's concern.
Summary of the invention
The preparation method that the bionical compacted zone/transition zone/weaker zone composite of a kind of outer fine and close (providing mechanics to support), internal layer hole non-uniform Distribution (being suitable for the soft or hard tissue ingrowth) is provided.By the structure of bionical body bone tissue, skin provides mechanics to support, and internal layer guiding soft or hard tissue ingrowth strengthens biocompatibility and forms mechanics to be fixed.And because the hole non-uniform Distribution of human body spongy bone, the porous layer of composite is designed to the compound requirement of satisfying non-uniform Distribution of transition zone and weaker zone.
A kind of method for preparation of pore heterogeneous distribution bionic bone material, it is raw material that the present invention adopts hydroxyapatite (HA) and Ti (or 316L) powder, adds plasticizer and pore creating material, outer fine and close, the internal layer pore heterogeneous distribution bionic bone material of preparation.Ti (or 316L) powder accounts for 5~30vol% of HA/Ti or HA/316L composite powder content, transition zone pore creating material content 30~60vol%, weaker zone pore creating material content 60~80vol%.In order to improve the powder sintered middle relatively poor shortcoming of binding ability of HA and Ti (or 316L), interpolation bio-vitric (BG) improves the bonding state between HA and the Ti interface, and the addition of bio-vitric is 0.5-2wt%.
Described pore heterogeneous distribution bionic bone material is made up of skin, transition zone and internal layer, and skin is a compacted zone, and internal layer is a weaker zone.
The gained material outer layer is HA/Ti or HA/316L composite compact layer, the intermediate layer is HA/Ti or the compound transition zone of HA/316L that porosity 38-60%, aperture 100-500 μ m account for 30-70%, and internal layer is HA/Ti or the compound weaker zone of HA/316L that porosity 57-80%, aperture 100-500 μ m account for 50-80%.
The preparation method of pore heterogeneous distribution bionic bone material is: after preparing HA/Ti (316L) composite powder or HA/BG/Ti (316L) composite powder in proportion, place on the mechanical type batch mixer, add the zirconia balls ball milling and mix, then cross 200 mesh sieves.With the powder that the makes diameter of packing into is the 25-30mm cylindrical mold, uses molybdenum sheet that the heterogeneity powder that is added is required to separate according to compacted zone/transition zone/weaker zone during the dress powder, and then press forming obtains pressed compact.(vacuum is 10 to carry out sintering under high vacuum condition
-2Pa), under 800 ℃ temperature, insulation certain hour (1-2h), the plasticizer and the pore creating material that are added when suppressing to remove.Then slowly be warming up to predetermined sintering temperature (1050-1250 ℃) again, insulation 1-2h.
In order to make forming effect better, the stearic acid that adds mass percent and be 0.5~1wt% in HA/Ti (316L) compound is as plasticizer.
Described pore creating material can be naphthalene, ammonium hydrogencarbonate or carbamide.
Among the present invention, the process of HA and respective amount Ti (or 316L) powder mixes can adopt ball milling method to carry out, and the time is preferably 4~12h.
The present invention is matrix with HA, with Ti powder or 316L powder is wild phase, with the bio-vitric is the bonding phase, with powder metallurgy vacuum sintering technique and molybdenum sheet separation method is manufacture method, the non-homogeneous distribution of pores characteristic of simulation body bone tissue, the non-homogeneous hole bionic bone material of preparation compacted zone/transition zone/weaker zone.Skin is a compacted zone, transition zone is HA/Ti or the compound transition zone of HA/316L that porosity 38-60%, aperture 100-500 μ m account for 30-70%, internal layer is HA/Ti or the compound weaker zone of HA/316L that porosity 57-80%, aperture 100-500 μ m account for 50-80%, and pore structure is the interconnected pore.The pore structure of biomaterial can satisfy the requirement of body bone tissue Haversian system 0~500 μ m pore-size substantially.Material of the present invention has superior biocompatibility and mechanical property concurrently, will have broad clinical application prospect aspect load-bearing bone reparation and the reconstruction.
Description of drawings
Fig. 1 is embodiment 1 a pore heterogeneous distribution bionic bone material dress mould sketch map, wherein: 1-weaker zone (internal layer); The 2-transition zone; 3-compacted zone (skin); The 4-mould inner wall;
Fig. 2 is embodiment 1 a sintered sample macroscopic view sketch map;
Fig. 3 is the hole cartogram of embodiment 1 transition zone;
Fig. 4 is the hole cartogram of embodiment 1 weaker zone;
Fig. 5 is embodiment 2 a sintered samples macroscopic view sketch map;
Fig. 6 is the hole cartogram of embodiment 2 transition zones;
Fig. 7 is the hole cartogram of embodiment 2 weaker zones;
Fig. 8 is embodiment 3 a sintered samples macroscopic view sketch map;
Fig. 9 is the hole cartogram of embodiment 3 transition zones;
Figure 10 is the hole cartogram of embodiment 3 weaker zones.
The specific embodiment
With HA powder, Ti powder, naphthalene, the stearic acid that makes, do not add pore creating material according to compacted zone, transition zone adds the 40vol% pore creating material, and weaker zone adds the method batching of 60vol% pore creating material, it is 15% that Ti accounts for HA/Ti composite powder content, and the content of stearic acid in composite powder is 0.8wt%.After preparing powder according to above ratio, be placed on the mechanical type batch mixer, add zirconia balls and mix 4h, 200 orders then sieve.So far, suppressing needed powder preparation finishes.
With the powder that makes dress mould, mould is cylindric (d=26mm), uses molybdenum sheet that the powder of the heterogeneity of being added is separated by Fig. 1 requirement during the dress powder.Adorn powder after separating, keep the vertically stable of molybdenum sheet in the dress powder process, pack the back into for cylindric at once to guarantee powder, after all powder has all been adorned, molybdenum sheet is slowly taken out the necessary careful operation of this process, in order to avoid cause the unordered mixing of powder, cause the failure of test.Dress is after powder finishes, and will sample be pressed places on the universal hydraulic testing machine to suppress, and pressure is decided to be 150MPa, in the pressing process, need put 150MPa place pressurize 30s at maximum pressure, and the demoulding then obtains pressed compact.(vacuum is 10 to carry out sintering at vacuum sintering furnace
-2Pa).With 5 ℃ of .min
-1Heating rate rise to 800 ℃, the insulation 1h, then with 10 ℃ of .min
-1Rise to 1200 ℃, insulation 2h.Should control heating rate slowly in the sintering process, cause crackle to produce to prevent material monolithic to be heated inhomogeneous and avoid the quick volatilization of pore creating material and cause the phenomenon of caving in of material.
Sample behind the sintering as shown in Figure 2.The photomacrograph of Fig. 2 the analysis showed that compacted zone, transition zone, the trilaminar gradient-structure of weaker zone form, and sample has higher-strength, and specimen surface does not have micro-crack to occur.
15%Ti non-homogeneous distribution of pores composite transition zone and weaker zone hole cumulative percentage can be listed cartogram, as Fig. 3 and Fig. 4.As shown in Figure 3, in the transition zone part, porosity is that the cumulative percentage of the hole of 38.5%, 0~100 μ m is that the hole cumulative percentage of 64.6%, 100~500 μ m is 35.4%.As shown in Figure 4, in the weaker zone part, porosity is that the shared percent of the hole of 63.5%, 0~100 μ m is that the shared percentage ratio of hole of 34.4%, 100~500 μ m is 65.6%.
According to body bone tissue Halffson system, the pore-size of osseous tissue is 0~500 μ m; As the timbering material of inducting osseous tissue growth, its best pore-size should be in 100~500 μ m.In conjunction with last surface analysis as can be known, the result of present embodiment can satisfy above-mentioned condition, and the weaker zone of sample and the hole non-uniform Distribution between the transition zone form.
Embodiment 2
With HA powder, 316L powder, ammonium hydrogencarbonate, the stearic acid that makes, do not add pore creating material according to compacted zone, transition zone adds the 40vol% pore creating material, weaker zone adds the method batching of 65vol% pore creating material, it is 25% that 316L accounts for HA/316L composite powder content, and the content of stearic acid in composite powder is 0.5wt%.After preparing powder according to above ratio, be placed on the mechanical type batch mixer, add zirconia balls and mix 8h, 200 orders then sieve.So far, suppressing needed powder preparation finishes.
With the powder that makes dress mould, mould is cylindric (d=25mm), uses molybdenum sheet that the powder of the heterogeneity of being added is separated by Fig. 1 requirement during the dress powder.Adorn powder after separating, keep the vertically stable of molybdenum sheet in the dress powder process, pack the back into for cylindric at once to guarantee powder, after all powder has all been adorned, molybdenum sheet is slowly taken out the necessary careful operation of this process, in order to avoid cause the unordered mixing of powder, cause the failure of test.Dress is after powder finishes, and will sample be pressed places on the universal hydraulic testing machine to suppress, and pressure is decided to be 200MPa, in the pressing process, need put 200MPa place pressurize 30s at maximum pressure, and the demoulding then obtains pressed compact.(vacuum is 10 to carry out sintering at vacuum sintering furnace
-2Pa), with 5 ℃ of .min
-1Heating rate rise to 800 ℃, the insulation 1.5h, then with 10 ℃ of .min
-1Rise to 1150 ℃, insulation 2h.Should control heating rate slowly in the sintering process, cause crackle to produce to prevent material monolithic to be heated inhomogeneous and avoid the quick volatilization of pore creating material and cause the phenomenon of caving in of material.
Sample behind the sintering as shown in Figure 5.The photomacrograph of Fig. 5 the analysis showed that compacted zone, transition zone, the trilaminar gradient-structure of weaker zone form, and sample has higher-strength, and specimen surface does not have micro-crack to occur.
25%316L non-homogeneous distribution of pores composite transition zone and weaker zone hole cumulative percentage can be listed cartogram, as Fig. 6 and Fig. 7.As shown in Figure 6, in the transition zone part, porosity is that the cumulative percentage of the hole of 42.4%, 0~100 μ m is that the cumulative percentage of the hole of 56.2%, 100~500 μ m is 43.8%.As shown in Figure 7, in the weaker zone part, porosity is that the shared percent of the hole of 67.5%, 0~100 μ m is that the shared percentage ratio of hole of 31.6%, 100~500 μ m is 68.4%.
According to body bone tissue Halffson system, the pore-size of osseous tissue is 0~500 μ m; As the timbering material of inducting osseous tissue growth, its best pore-size should be in 100~500 μ m.In conjunction with last surface analysis as can be known, the result of present embodiment can satisfy above-mentioned condition, and the weaker zone of sample and the hole non-uniform Distribution between the transition zone form.
Embodiment 3
With HA powder, Ti powder, biological glass powder, naphthalene, the stearic acid that makes, do not add pore creating material according to compacted zone, transition zone adds the 55vol% pore creating material, weaker zone adds the method batching of 75vol% pore creating material, it is 8% that Ti accounts for HA/Ti composite powder content, the content of stearic acid in composite powder is 0.6wt%, and the content of bio-vitric in composite powder is 0.8wt%.After preparing powder according to above ratio, be placed on the mechanical type batch mixer, add zirconia balls and mix 3h, 200 orders then sieve.So far, suppressing needed powder preparation finishes.
With the powder that makes dress mould, mould is cylindric (d=28mm), uses molybdenum sheet that the powder of the heterogeneity of being added is separated by Fig. 1 requirement during the dress powder.Adorn powder after separating, keep the vertically stable of molybdenum sheet in the dress powder process, pack the back into for cylindric at once to guarantee powder, after all powder has all been adorned, molybdenum sheet is slowly taken out the necessary careful operation of this process, in order to avoid cause the unordered mixing of powder, cause the failure of test.Dress is after powder finishes, and will sample be pressed places on the universal hydraulic testing machine to suppress, and pressure is decided to be 300MPa, in the pressing process, need put 300MPa place pressurize 30s at maximum pressure, and the demoulding then obtains pressed compact.(vacuum is 10 to carry out sintering at vacuum sintering furnace
-2Pa), with 5 ℃ of .min
-1Heating rate rise to 800 ℃, the insulation 1h, then with 10 ℃ of .min
-1Rise to 1100 ℃, insulation 2h.Should control heating rate slowly in the sintering process, cause crackle to produce to prevent material monolithic to be heated inhomogeneous and avoid the quick volatilization of pore creating material and cause the phenomenon of caving in of material.
Sample behind the sintering as shown in Figure 8.The photomacrograph of Fig. 8 the analysis showed that compacted zone, transition zone, the trilaminar gradient-structure of weaker zone form, and sample also has higher-strength, and specimen surface does not have micro-crack to occur.
8%Ti non-homogeneous distribution of pores composite transition zone and weaker zone hole cumulative percentage can be listed cartogram, as Fig. 9 and Figure 10.As shown in Figure 9, in the transition zone part, porosity is that the cumulative percentage of the hole of 58.8%, 0~100 μ m is that the cumulative percentage of the hole of 64.6%, 100~500 μ m is 35.4%.As shown in figure 10, in the weaker zone part, porosity is that the shared percent of the hole of 78.4%, 0~100 μ m is that the shared percentage ratio of hole of 34.4%, 100~500 μ m is 65.6%.
According to body bone tissue Halffson system, the pore-size of osseous tissue is 0~500 μ m; As the timbering material of inducting osseous tissue growth, its best pore-size should be in 100~500 μ m.In conjunction with last surface analysis as can be known, the result of present embodiment can satisfy above-mentioned condition, and the weaker zone of sample and the hole non-uniform Distribution between the transition zone form.
Claims (6)
1. method for preparation of pore heterogeneous distribution bionic bone material is characterized in that:
(1) described pore heterogeneous distribution bionic bone material is made up of skin, transition zone and internal layer, and skin is a compacted zone, and internal layer is a weaker zone;
(2) the preparation raw material of described pore heterogeneous distribution bionic bone material is that hydroxyapatite is HA and Ti or 316L powder, and Ti or 316L powder account for 5~30vol% of HA/Ti or HA/316L composite powder content;
(3) when mixing, material powder adds pore creating material, transition zone material powder pore creating material content 30~60vol%, weaker zone material powder pore creating material content 60~80vol%;
(4) material powder is crossed 200 mesh sieves behind ball milling, and the cylindrical mold of packing into uses molybdenum sheet that powder is separated according to compacted zone/transition zone/weaker zone during the dress powder, and then press forming obtains pressed compact; Pressed compact carries out sintering under high vacuum condition, sintering vacuum is 10
-2Pa, under 800 ℃ temperature, insulation 1-2h slowly is warming up to sintering temperature 1050-1250 ℃ again, insulation 1-2h;
2. method according to claim 1 is characterized in that: adding mass percent in material powder is the bio-vitric of 0.5-2%.
3. method according to claim 1 is characterized in that: add mass percent and be 0.5~1% stearic acid in material powder as plasticizer.
4. method according to claim 1 is characterized in that: described pore creating material is naphthalene, ammonium hydrogencarbonate or carbamide.
5. method according to claim 1 is characterized in that: described cylindrical mold diameter is 25-30mm.
6. method according to claim 1 is characterized in that: the described ball milling time is 4~12h.
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