CN204601180U - A kind of gradient-structure calcium phosphate biological ceramic - Google Patents
A kind of gradient-structure calcium phosphate biological ceramic Download PDFInfo
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- CN204601180U CN204601180U CN201420850174.2U CN201420850174U CN204601180U CN 204601180 U CN204601180 U CN 204601180U CN 201420850174 U CN201420850174 U CN 201420850174U CN 204601180 U CN204601180 U CN 204601180U
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Abstract
The utility model discloses a kind of gradient-structure calcium phosphate biological ceramic, described material comprises three kinds of different gradient crystal structure layer such as nanocrystalline structure surface layer, Nano/micron crystal structure transition zone, micro-crystal structure centre layer.Described material obtains the pottery with nanometer, the change of micro-crystal gradient-structure by setting up sintering temperature Gradient distribution field.The nanocrystal layer of material gives the biological activity of material uniqueness, micro-crystal layer ensures the mechanical property of material, therebetween gradient transition, combine closely, and combine the mechanical property with matching materials and natural sclerous tissues by adjustment Nano/micron Rotating fields, thus meet the multi-functional demand object of biomaterial.
Description
Technical field
This utility model belongs to field of biomedical materials, is specifically related to a kind of gradient-structure calcium phosphate biological ceramic.
Background technology
Desirable hard tissue repair biomaterial should have both the multi-functional requirements such as good biological characteristics and mechanical characteristic simultaneously.Biology performance mainly wishes that it has good biocompatibility, bone conductibility, osteoinductive and degradable, absorbability.Mechanical property comprises resistance to compression, bending strength, multiple aggregative indicator such as elastic modelling quantity should to greatest extent close to or match with the mechanical property of nature bone.
Existing research is thought, the chemical composition of material, interface and microstructure have decision meaning to its biological characteristics sexual function.Nano meter biomaterial due to the uniqueness " nano effect " that has and " interface feature ", as the characteristics such as small-size effect, high-specific surface area, surface/interface effect have tempting application prospect in hard tissue engineering field of repairing.Calcium phosphate and the natural sclerous tissues of nanoscale have further similarity on chemical composition, structure and yardstick, and the crystal grain in nano meter biomaterial, crystal boundary and combination thereof are all in nano-scale.Grain refinement, number of grain boundaries increases considerably, and effectively can improve the interface alternation effect between material and biotic environment, promotes the absorption of associated protein, cell and sticks, thus makes the excellent biology performance of nano meter biomaterial tool.At present, although have numerous in synthesis, preparation and the research report evaluating nano-calcium phosphate material, but in the materials application that it is concrete, nano-calcium phosphate mostly in a dispersed form, as solution particulates, colloid, or with the form doped and compounded of second-phase among other matrix materials (as macromolecular material, collagen etc.).But the nano-calcium phosphate material preparing block shape is still a large technical barrier because its sintering process restricts.In material sintering process, along with temperature rising and the prolongation of time, the mutual welding of nano-solid granule, crystal boundary merges minimizing gradually, easily causes material grains to be grown up, thus cannot obtain the calcium phosphate ceramic material of nanocrystal.From technique itself, the preparation flow of nano ceramics there is no too large difference with conventional ceramic, generally follows the operation of powder body-molding-sintering, but from technical application level face, the technology of preparing of nano ceramics is extremely harsh.
Meeting on the multi-functional property requirements of hard tissue repair biomaterial, the design of FGM (Functionally graded materials, FGM) has huge advantage.The concept of function-graded material by Japanese Xinye just wait scholar first to propose in 1987 with the quick hero of horizontal well, the design of material thought of functionally gradient used for reference by functionally gradient biomaterial, by the component to material, structural design, make material different parts have different functional performances, thus make material monolithic show multiple functional characteristic to meet the multi-functional requirement of biomaterial.Up to now, people have explored some basic research methoies, prepare some gradient function biomaterials and achieve certain effect, but existing gradient function biomaterial is all metal-ceramic FGM substantially.This kind of metal-ceramic FGM in clinical practice, ubiquity coating and substrate bond strength is inadequate, coating degradation easily makes the metallic substrates problem such as exposed again.Therefore, the gradient function biomaterial of a new generation still awaits further optimized development, to meet the multi-functional characteristic requirements of biomaterial and reliable, safe object.
Utility model content
The purpose of this utility model is the multi-functional HA calcium phosphate biological ceramic of a kind of gradient-structure developed for the deficiencies in the prior art.Be characterized in obtaining the bioceramic with nanometer, micro-crystal graded structure by setting up sintering temperature Gradient distribution field.
This utility model is achieved through the following technical solutions:
A kind of gradient-structure calcium phosphate biological ceramic, comprises nanocrystalline structure layer, Nano/micron crystal structure transition zone, micro-crystal structure sheaf.The mechanics function constant gradient functional characteristic that described material has good biological function simultaneously, matches with natural bone tissue.Nanocrystalline structure layer in material gives the biological activity of material uniqueness, guarantee special functional demands biology of material, promote that material and biological tissue interface are formed, strengthen bone to connect and healing function, micro-crystal structure sheaf ensures the mechanical property of material, and by regulating the structural grouping of nanocrystalline structure layer and micro-crystal structure sheaf with the mechanical property of matching materials and natural sclerous tissues, thus meet the multi-functional demand object of biomaterial, make to combine between bioactive layer and mechanical property ergosphere closely by described Nano/micron crystal structure transition zone, can not be peeling in use procedure, the phenomenons such as layering comes off.
Alternately, in above-mentioned gradient-structure calcium phosphate biological ceramic, carry out continuous gradient ground transition by Nano/micron crystal structure transition zone between nanocrystalline structure layer with micro-crystal structure sheaf and be connected, between layers without obvious boundary.
Alternately, in above-mentioned gradient-structure calcium phosphate biological ceramic, described calcium phosphate is at least one in hydroxyapatite, tricalcium phosphate, biphasic calcium phosphate, element doping modified phosphate calcium.
Alternately, in above-mentioned gradient-structure calcium phosphate biological ceramic, described material has nucleocapsid structure, is respectively micro-crystal structure centre layer, Nano/micron crystal structure transition zone, nanocrystalline structure surface layer from inside to outside.
Alternately, in above-mentioned gradient-structure calcium phosphate biological ceramic, described material has three-decker, is respectively micro-crystal structure sheaf at two ends and nanocrystalline structure layer and the Nano/micron crystal structure transition zone between described micro-crystal structure sheaf and nanocrystalline structure layer.。
Alternately, in above-mentioned gradient-structure calcium phosphate biological ceramic, described material has five-layer structure, two the Nano/micron crystal structure transition zones being respectively a micro-crystal structure centre layer at center and two nanocrystalline structure surface layers on material two-side top layer and laying respectively between described central core and surface layer.
Alternately, in above-mentioned gradient-structure calcium phosphate biological ceramic, in the crystal structure distribution of described material, the percentage ratio of each layer thickness is, nanocrystalline structure layer: 1% ~ 20%, Nano/micron crystal structure transition zone: 10% ~ 30%, micro-crystal structure sheaf: 89% ~ 50%.
Alternately, in above-mentioned gradient-structure calcium phosphate biological ceramic, the nanocrystalline structure layer of described material mainly crystal grain diameter is the calcium phosphate polycrystal of 80 ~ 100nm.Further, wherein nanocrystalline crystal grain has irregular pattern, without obvious crystal boundary between crystal grain.
Alternately, in above-mentioned gradient-structure calcium phosphate biological ceramic, described Nano/micron crystal structure transition zone mainly crystal grain diameter is the calcium phosphate polycrystal of 100 ~ 1000nm.Further, nanocrystallinely in described transition zone to mix with micron crystalline substance, crystal grain has irregular pattern, without obvious crystal boundary between crystal grain.
Alternately, in above-mentioned gradient-structure calcium phosphate biological ceramic, described micro-crystal structure sheaf mainly crystal grain diameter is the calcium phosphate polycrystal of 1 ~ 5 μm.Further, wherein the crystal grain of micron crystalline substance has irregular pattern, has obvious crystal boundary between crystal grain.
All features disclosed in this description, or the step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.
The beneficial effects of the utility model:
1, this utility model gives bioceramic enough mechanical properties, the maximum compressive strength of material is about 67 ~ 136MPa, suitable with human body compact bone intensity, and the mechanical property of material can by its gradient-structure of adjustment ideally to mate the biomechanics requirement of human body hard tissue.
2, gradient-structure calcium phosphate biological ceramic described in the utility model has nanocrystalline structure surface, the surface/interface of material has comparatively bigger serface, be beneficial to absorption skeletonization associated protein and cell, be easy to material and discharge calcium, phosphonium ion fast in vivo, promote New born formation, give the good biocompatibility of HA bioceramic and biological activity, guarantee special functional demands biology of material, promote that material and biological tissue interface are formed, strengthen bone and connect and healing function;
3, this utility model has multi-functional material result, and is gradient transition structure between each functional layer, combines closely, there is not the problem of stripping, layering between bioactive layer and mechanical property ergosphere.
Accompanying drawing explanation
Fig. 1. the nano HA microgranule transmission electron microscope picture of synthesis in embodiment 1;
Fig. 2. the structural representation of gained gradient bioceramic in embodiment 1, wherein (a) is the partial cut-away structural representation of function gradient structure HA bioceramic, b nanocrystalline structure layer SEM that () is function gradient structure HA bioceramic schemes, c micro-crystal structure sheaf SEM that () is function gradient structure HA bioceramic schemes, and the transition zone SEM that (d) is function gradient structure HA bioceramic schemes;
Fig. 3. the XRD figure spectrum of gained sample in embodiment 1, wherein (a) is multi-functional HA bioceramic phase constituent qualification XRD figure of the present invention, and (b) is HA crystal standard XRD pattern;
Fig. 4. the Mechanics Performance Testing figure of multifunctional gradient structure HA bioceramic;
Fig. 5. the burnt photo of light copolymerization of material and co-culture of cells, wherein (a) is conventional H A pottery mesenchymal stem cells MSCs (MSCs) In vitro culture 1 day laser co-focusing figure, b () is conventional H A pottery mesenchymal stem cells MSCs (MSCs) In vitro culture 4 days laser co-focusing figure, c () is conventional H A pottery mesenchymal stem cells MSCs (MSCs) In vitro culture 7 days laser co-focusing figure, d () is embodiment 5 mesenchymal stem cells MSCs (MSCs) the In vitro culture laser co-focusing figure of 1 day, e () is embodiment 5 mesenchymal stem cells MSCs (MSCs) the In vitro culture laser co-focusing figure of 4 days, f () is embodiment 5 mesenchymal stem cells MSCs (MSCs) the In vitro culture laser co-focusing figure of 7 days,
Fig. 6. the structural representation with the calcium phosphate biological ceramic of three-decker described in the utility model;
Fig. 7. the cross section structure schematic diagram with post Rotating fields calcium phosphate biological ceramic described in the utility model.
Reference numeral: 1 be nanocrystalline structure layer, 2 be Nano/micron crystal structure transition zone, 3 for micro-crystal structure sheaf.
Detailed description of the invention
By the following examples this utility model is specifically described; what be necessary to herein means out is that the present embodiment is only for being further described this utility model; but can not be interpreted as the restriction to this utility model protection domain, the person skilled in the art in this field can make improvement and the adjustment of some non-intrinsically safes to this utility model according to above-mentioned content of the present utility model.
embodiment 1:
1) by " wet chemistry reaction " synthesis of nano hydroxyapatite (HA) microgranule, synthesis material is diammonium hydrogen phosphate and lime nitrate, synthetic solvent system pH is adjusted to 7.4-8.0 by ammonia, nano HA microgranule after synthesis is through leaving standstill, ageing, and repeatedly cleaning 3 times by deionized water, precipitate is filtered through low-temperature air-drying, and HA mean particle dia is 30 ~ 60nm;
2) base substrate makes: among the polyvinyl alcohol Homogeneous phase mixing of 2wt% to nanometer hydroxyapatite forerunner powder, accurate weighing 1g mixed powder is also poured in cylindrical stainless steel mould, by vertical hydraulic formula " isostatic compaction " press ceramic green compact, pressure is kept to be 6MPa in pressing process, dwell time is 15 seconds, and obtains ceramic green rolled-up stock by ejection device;
3) embed: the embedding sintering system of setting up surrounding, ceramic body is placed in round alumina ceramic crucible, surrounding uniform thickness covers Al
2o
3embedded material, embedded material thickness is 10 times of ceramic body external diameter, natural compacting;
4) sinter, embedding sintered body is put into vacuum drying oven and sinters, adopt two-step method, with the speed rapid temperature increases to 700 DEG C of 10 DEG C/min, after reaching critical crystal temperature, be cooled to rapidly 600 DEG C, be incubated 10 hours, then furnace cooling.
Structural characterization and performance test:
1, ceramics precursor diameter of particle is tested by TEM and is characterized.
Shown in Fig. 1.
Result shows: this synthetic powder is the nanoparticle of grain of rice shape, and mean particle dia is about 30 ~ 60nm, and draw ratio is 1:1 ~ 5:1.
2, the microstructure of ceramic material is tested through SEM.
The section of scanning electron microscope to gained ceramic material is adopted to observe, shown in Fig. 2 (a) ~ (d).
Result shows: the two-sided shallow surface structure of material is nanocrystalline structure, and its HA crystal diameter is 80 ~ 100nm;
The transition layer structure of material occupy below double-faced surface, and be Nano/micron HA crystal hybrid architecture, diameter is 100 ~ 1000nm; The intermediate layer of material is micro-crystal structure, and its HA crystal diameter is 0.5 ~ 5 μm.
3, the phase constituent of material is identified by XRD and is characterized.
Shown in Fig. 3 (a) ~ (b).
Result shows: material is hydroxyapatite crystal.
4, material mechanical performance is through dynamic mechanical test (Dynamic mechanical analysis, DMA).
Shown in Fig. 4.
Result shows: by regulating the thickness combination in the sample of Nano/micron layer, the mechanical property of ceramic material roughly can be mated with the mechanical property of natural sclerous tissues, and its maximum compressive strength numerical value is 67 ~ 136MPa.
5, the biology function characteristic of material cultivates test by external mesenchymal stem cells MSCs (MSCs).
Shown in Fig. 5 (a) ~ (f).
Result shows: multifunctional gradient structure HA bioceramic has good biocompatibility, compares conventional micron crystal HA pottery and has better biological activity, can promote the differentiation of mesenchymal stem cells MSCs, propagation and growth.
The gradient-structure HA bioceramic of gained is outwards presented the crystal structure (having nucleocapsid structure) of 3 different levels successively by center, the scanning electron microscopic picture of its cut-away section as shown in Figure 2.Can see from SEM figure, the two-sided shallow surface structure of material is nanocrystalline structure, and its HA crystal diameter is 80 ~ 90nm; The transition layer structure of material occupy below double-faced surface, and be Nano/micron HA crystal hybrid architecture, diameter is 90 ~ 500nm; The intermediate layer of material is micro-crystal structure, and its HA crystal diameter is 0.5 ~ 1.8 μm.
By adjusting the shape of base substrate, and after having sintered, suitable cutting is carried out to material, obtain respectively having three-decker (as Fig. 6) and five-layer structure (as in Fig. 2 a) and the gradient-structure HA bioceramic of post Rotating fields (schematic cross-section is as Fig. 7).
embodiment 2:
Be that the HA powder of 50 ~ 80nm is for raw material with mean particle dia, evenly be mixed into the polyvinyl alcohol of 2wt%, accurate weighing 1g mixed powder, by vertical hydraulic formula " isostatic compaction " method press ceramic green compact, in pressing process, pressure is 6MPa, dwell time is 15 seconds, has the HA bioceramic of gradient-structure by setting up different sintering temperature gradient fields sintering.Its product preparation process and step identical with embodiment 1, difference is to adopt different critical sintering temperatures in step 4 sintering process, namely in two-step method, the first step is with the speed rapid temperature increases to 750 DEG C of 10 DEG C/min, then 500 DEG C are cooled to rapidly, be incubated 10 hours, then furnace cooling.The HA pottery material of gained still presents the crystal structure of 3 different levels, and wherein the two-sided shallow surface structure of material is nanocrystalline structure, and HA crystal diameter is 80 ~ 90nm; Transition layer structure is Nano/micron HA crystal hybrid architecture, and HA crystal diameter is 90 ~ 800nm; The central core of material is micro-crystal structure, and HA crystal diameter is 0.8 ~ 2.5 μm.This is because higher critical sintering temperature changes the Gradient distribution of sintering temperature field, thus obtain larger HA crystalline size.
embodiment 3:
With mean particle dia be the HA powder of 50 ~ 80nm for raw material, preparation has the HA bioceramic of gradient-structure.Its product preparation process and step identical with embodiment 1, difference is to adopt different critical sintering temperatures in step 4 sintering process, namely in two-step method, the first step is with the speed rapid temperature increases to 800 DEG C of 10 DEG C/min, then 600 DEG C are cooled to rapidly, be incubated 10 hours, then furnace cooling.The HA pottery material of gained still presents the crystal structure of 3 different levels, and wherein the two-sided shallow surface structure of material is nanocrystalline structure, and HA crystal diameter is 80 ~ 95nm; Transition layer structure is Nano/micron HA crystal hybrid architecture, and HA crystal diameter is 95 ~ 1000nm; The central core of material is micro-crystal structure, and HA crystal diameter is 1.0 ~ 3.5 μm.This is because higher critical sintering temperature changes the Gradient distribution of sintering temperature field, thus obtain larger HA crystalline size.
embodiment 4:
With mean particle dia be the HA powder of 50 ~ 80nm for raw material, preparation has the HA bioceramic of gradient-structure.Its product preparation process and step identical with embodiment 1, difference is to adopt different critical sintering temperatures in step 4 sintering process, namely in two-step method, the first step is with the speed rapid temperature increases to 850 DEG C of 10 DEG C/min, then 600 DEG C are cooled to rapidly, be incubated 10 hours, then furnace cooling.The HA pottery material of gained still presents the crystal structure of 3 different levels, and wherein the two-sided shallow surface structure of material is nanocrystalline structure, and HA crystal diameter is 80 ~ 100nm; Transition layer structure is Nano/micron HA crystal hybrid architecture, and HA crystal diameter is 100 ~ 1500nm; The central core of material is micro-crystal structure, and HA crystal diameter is 1.5 ~ 4.5 μm.This is because higher critical sintering temperature changes the Gradient distribution of sintering temperature field, thus obtain larger HA crystalline size.
embodiment 5:
Be that the HA powder of 50 ~ 80nm is for raw material with mean particle dia, evenly be mixed into the polyvinyl alcohol of 2wt%, accurate weighing 1g mixed powder, by vertical hydraulic formula " isostatic compaction " method press ceramic green compact, in pressing process, pressure is 6MPa, dwell time is 15 seconds, sets up by changing embedded material the HA bioceramic that different sintering temperature gradient fields sintering has gradient-structure.Other technique is with used identical in embodiment 1, and difference is to adopt different embedded materials, and this example adopts MgO to embed ceramic body and sinters.The HA pottery material of gained still presents the crystal structure of 3 different levels, wherein the two-sided shallow surface structure of material is nanocrystalline structure (5% ~ 1%), transition layer structure is Nano/micron HA crystal hybrid architecture (20% ~ 10%), the central core of material is micro-crystal structure (75 ~ 89%), and all types of crystal structure layer distributions of material there occurs change.This is because different embedded materials has the different coefficients of heat conduction, thus change the Gradient distribution of sintering temperature field, obtain the HA pottery with the distribution of different crystal structure sheaf.
embodiment 6:
Its product preparation process and step identical with process example 5, difference be this example adopt SiO
2embedding ceramic body sinters.The HA pottery material of gained still presents the crystal structure of 3 different levels, wherein the two-sided shallow surface structure of material is nanocrystalline structure (10% ~ 1%), transition layer structure is Nano/micron HA crystal hybrid architecture (30% ~ 10%), the central core of material is micro-crystal structure (60 ~ 89%), and all types of crystal structure layer distributions of material there occurs change.This is because different embedded materials has the different coefficients of heat conduction, thus change the Gradient distribution of sintering temperature field, obtain the HA pottery with the distribution of different crystal structure sheaf.
embodiment 7:
Product preparation process and step identical with embodiment 1, choosing HA pottery material is the crystal structure with 3 different levels, the two-sided shallow surface structure of its material is nanocrystalline structure, shared section thickness is: 1% ~ 7%, transition layer structure is Nano/micron HA crystal hybrid architecture, shared section thickness is: 10% ~ 17%, the central core of material is micro-crystal structure, shared section thickness is: 89 ~ 76%, tested by material dynamic mechanical, the maximum compressive strength recording material is: 136 ± 13MPa.Because different HA crystal structures has different mechanical properties, by changing the different crystal structure percentage composition of ceramic material, the adjustment to material mechanical performance can be realized.
embodiment 8:
Product preparation process and step identical with embodiment 1, choosing HA pottery material is the crystal structure with 3 different levels, the two-sided shallow surface structure of its material is nanocrystalline structure, shared section thickness is: 7% ~ 14%, transition layer structure is Nano/micron HA crystal hybrid architecture, shared section thickness is: 17% ~ 24%, the central core of material is micro-crystal structure, shared section thickness is: 76 ~ 62%, tested by material dynamic mechanical, the maximum compressive strength recording material is 103 ± 12MPa: because different HA crystal structures has different mechanical properties, by changing the different crystal structure percentage composition of ceramic material, the adjustment to material mechanical performance can be realized.
embodiment 9:
Product preparation process and step identical with embodiment 1, choosing HA pottery material is the crystal structure with 3 different levels, the two-sided shallow surface structure of its material is nanocrystalline structure, shared section thickness is: 14% ~ 20%, transition layer structure is Nano/micron HA crystal hybrid architecture, shared section thickness is: 24% ~ 30%, the central core of material is micro-crystal structure, shared section thickness is: 62 ~ 50%, tested by material dynamic mechanical, the maximum compressive strength recording material is: 67 ± 10MPa.Because different HA crystal structures has different mechanical properties, by changing the different crystal structure percentage composition of ceramic material, the adjustment to material mechanical performance can be realized.
embodiment 10:
Respectively using the nano powder of the HA of β tricalcium phosphate, biphasic calcium phosphate, doping strontium element as forerunner's powder, sinter in sintering temperature Gradient distribution field described in the utility model after body preparation, successfully prepared corresponding gradient-structure calcium phosphate biological ceramic respectively, resulting materials comprises nanocrystalline structure layer, Nano/micron crystal structure transition zone, micro-crystal structure sheaf.Wherein the calcium phosphate polycrystal thickness of nanocrystalline structure layer to be crystal grain diameter be 80 ~ 100nm accounts for 1% ~ 20% of gross thickness, the calcium phosphate polycrystal of Nano/micron crystal structure transition zone to be crystal grain diameter be 100 ~ 1000nm, thickness accounts for 10% ~ 30%, and to be crystal grain diameter be micro-crystal structure sheaf that the calcium phosphate polycrystal thickness of 1 ~ 5 μm accounts for 89% ~ 50%.
application example 1:
Be that the HA powder of 50 ~ 80nm is for raw material with mean particle dia, evenly be mixed in polyvinyl alcohol to the 1 gram HA powder of 2wt%, by vertical hydraulic formula " isostatic compaction " method press ceramic green compact, pressing pressure is 6MPa, dwell time is 15 seconds, its product preparation process and step identical with embodiment 1, difference is to adopt conventional one-step method sintered ceramic in step 4 sintering process, namely in sintering process, directly with the speed rapid temperature increases to 1100 DEG C of 10 DEG C/min, be incubated 10 hours, then furnace cooling.The micro-crystal of gained pottery is carried out mesenchymal stem cells MSCs (MSCs) In vitro culture 7 days as substrate, result as shown in Figure 5, MSCs is attached at ceramic surface growth, cell population upgrowth situation is good, obtain certain proliferation and differentiation, illustrate that HA ceramic material has good biocompatibility.
application example 2:
Be that the HA powder of 50 ~ 80nm is for raw material with mean particle dia, evenly be mixed in polyvinyl alcohol to the 1 gram HA powder of 2wt%, by vertical hydraulic formula " isostatic compaction " method press ceramic green compact, pressing pressure is 6MPa, dwell time is 15 seconds, its product preparation process and step identical with Application Example 1, difference is to adopt in step 4 sintering process two-step method to build the distribution of sintering temperature gradient fields, and concrete sintering parameter is as described in example 2 above.The gradient-structure HA pottery with nano topography feature of gained is carried out mesenchymal stem cells MSCs (MSCs) In vitro culture 4 days as substrate, result is as shown in Fig. 5-e, MSCs in ceramic surface overall growth in order, obtain certain differentiation and proliferation, compare the micron surface pottery of same incubation time point, this gradient function HA ceramic material has better biological activity.
application example 3:
Gradient function HA pottery is prepared with the method described in Application Example 2, all parameters and preparation process are as Application Example 2, difference is this gradient-structure HA pottery to cultivate MSCs to 7 day as substrate, result is as shown in Fig. 5-f, MSCs ceramic surface attaching in order, cell proliferation is obvious, extend in material surface differentiation, connect into the network-like structure of plane gradually, the upgrowth situation of cell is good, the micron surface pottery that propagation compares same incubation time point is more obvious, and this gradient function HA ceramic material has better biological activity.
The foregoing is only preferred embodiment of the present utility model, is only illustrative for this utility model, and nonrestrictive; Those of ordinary skill in the art understand, and can carry out many changes in the spirit and scope that this utility model limits to it, amendment, and even equivalence is changed, but all will fall into protection domain of the present utility model.
Claims (8)
1. a gradient-structure calcium phosphate biological ceramic, is characterized in that, comprises nanocrystalline structure layer, Nano/micron crystal structure transition zone, micro-crystal structure sheaf.
2. calcium phosphate biological ceramic according to claim 1, it is characterized in that, in the crystal structure distribution of described bioceramic, the percentage ratio of each layer thickness is, nanocrystalline structure layer: 1% ~ 20%, Nano/micron crystal structure transition zone: 10% ~ 30%, micro-crystal structure sheaf: 89% ~ 50%.
3. calcium phosphate biological ceramic according to claim 1, is characterized in that, described bioceramic has nucleocapsid structure, is respectively micro-crystal structure centre layer, Nano/micron crystal structure transition zone, nanocrystalline structure surface layer from inside to outside.
4. calcium phosphate biological ceramic according to claim 1, it is characterized in that, described bioceramic has three-decker, is respectively micro-crystal structure sheaf at two ends and nanocrystalline structure layer and the Nano/micron crystal structure transition zone between described micro-crystal structure sheaf and nanocrystalline structure layer.
5. calcium phosphate biological ceramic according to claim 1, it is characterized in that, described bioceramic has five-layer structure, two the Nano/micron crystal structure transition zones being respectively a micro-crystal structure centre layer at center and two nanocrystalline structure surface layers on material two-side top layer and laying respectively between described central core and surface layer.
6. calcium phosphate biological ceramic according to claim 1, is characterized in that, the nanocrystalline structure layer of described bioceramic mainly crystal grain diameter is the calcium phosphate polycrystal of 80 ~ 100nm.
7. calcium phosphate biological ceramic according to claim 1, is characterized in that, described Nano/micron crystal structure transition zone mainly crystal grain diameter is the calcium phosphate polycrystal of 100 ~ 1000nm.
8. calcium phosphate biological ceramic according to claim 1, is characterized in that, described micro-crystal structure sheaf mainly crystal grain diameter is the calcium phosphate polycrystal of 1 ~ 5 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104491923A (en) * | 2014-12-26 | 2015-04-08 | 四川大学 | Nanometer/micrometer-crystal gradient structure calcium phosphate bio-ceramic material as well as preparation method and application thereof |
| CN108379665A (en) * | 2018-03-12 | 2018-08-10 | 四川大学 | A kind of artificial neural plate and preparation method thereof of double gradients |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104491923A (en) * | 2014-12-26 | 2015-04-08 | 四川大学 | Nanometer/micrometer-crystal gradient structure calcium phosphate bio-ceramic material as well as preparation method and application thereof |
| CN106187147A (en) * | 2014-12-26 | 2016-12-07 | 四川大学 | Nano/micron crystal gradient-structure calcium phosphate biological ceramic material and application thereof |
| CN106187147B (en) * | 2014-12-26 | 2019-01-15 | 四川大学 | Nano/micron crystal gradient-structure calcium phosphate biological ceramic material and its application |
| CN108379665A (en) * | 2018-03-12 | 2018-08-10 | 四川大学 | A kind of artificial neural plate and preparation method thereof of double gradients |
| CN108379665B (en) * | 2018-03-12 | 2020-11-03 | 四川大学 | Double-gradient artificial vertebral plate and preparation method thereof |
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