CN103058707B - Beta-dicalcium silicate porous biological ceramic bracket and preparation method and application thereof - Google Patents
Beta-dicalcium silicate porous biological ceramic bracket and preparation method and application thereof Download PDFInfo
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- CN103058707B CN103058707B CN201210528010.3A CN201210528010A CN103058707B CN 103058707 B CN103058707 B CN 103058707B CN 201210528010 A CN201210528010 A CN 201210528010A CN 103058707 B CN103058707 B CN 103058707B
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- 229910052918 calcium silicate Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000919 ceramic Substances 0.000 title abstract description 8
- 210000000988 bone and bone Anatomy 0.000 claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 16
- 239000006260 foam Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000003462 bioceramic Substances 0.000 claims description 37
- 238000000498 ball milling Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
- 238000010304 firing Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 210000001519 tissue Anatomy 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 4
- 230000011218 segmentation Effects 0.000 claims description 4
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 4
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 2
- 210000004027 cell Anatomy 0.000 description 27
- 239000000463 material Substances 0.000 description 17
- 239000001506 calcium phosphate Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 229940078499 tricalcium phosphate Drugs 0.000 description 5
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 5
- 235000019731 tricalcium phosphate Nutrition 0.000 description 5
- 239000011575 calcium Substances 0.000 description 4
- 238000004113 cell culture Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 230000012010 growth Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000004071 biological effect Effects 0.000 description 3
- 239000012620 biological material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 210000002744 extracellular matrix Anatomy 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 102000010834 Extracellular Matrix Proteins Human genes 0.000 description 2
- 108010037362 Extracellular Matrix Proteins Proteins 0.000 description 2
- 230000000680 avirulence Effects 0.000 description 2
- 235000012241 calcium silicate Nutrition 0.000 description 2
- JHLNERQLKQQLRZ-UHFFFAOYSA-N calcium silicate Chemical compound [Ca+2].[Ca+2].[O-][Si]([O-])([O-])[O-] JHLNERQLKQQLRZ-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000004069 differentiation Effects 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 210000000056 organ Anatomy 0.000 description 2
- 210000000963 osteoblast Anatomy 0.000 description 2
- 230000002138 osteoinductive effect Effects 0.000 description 2
- 201000008968 osteosarcoma Diseases 0.000 description 2
- 230000002629 repopulating effect Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- -1 ammonia ester Chemical class 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 210000001185 bone marrow Anatomy 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000024245 cell differentiation Effects 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 210000001612 chondrocyte Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000001582 osteoblastic effect Effects 0.000 description 1
- 210000004409 osteocyte Anatomy 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 210000000130 stem cell Anatomy 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000005287 template synthesis Methods 0.000 description 1
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/10—Ceramics or glasses
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
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- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/22—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in calcium oxide, e.g. wollastonite
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
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- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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Abstract
The invention discloses a beta-dicalcium silicate porous biological ceramic bracket and a preparation method and an application thereof. The preparation method of the beta-dicalcium silicate porous biological ceramic bracket comprises the following steps: adopting porous organic foam as a precursor; adding the foam precursor in ceramic slurry for impregnating and slurry hanging after treatment; drying and firying after removing spare ceramic slurry so as to manufacture the beta-dicalcium silicate porous biological ceramic bracket. The biological ceramic bracket is good in through hole property, mechanical performance and biological compatibility, and can be applied to bone tissue engineering.
Description
Technical field
The present invention includes a kind of bone tissue engineer biologic bracket material and its preparation method and application, relate in particular to a kind of bioceramic scaffold and its preparation method and application.
Background technology
Organizational project is the principle of application cell biology, biomaterial and engineering, and research and development are for the cross discipline of the biological activity substitute of the structure of gentrify human body disease damage tissue or organ, function.Its research mainly comprises three aspects: seed cell, biomaterial scaffolds and growth signals.Biologic bracket material is the key factor of organizational project, thereby exploitation builds research emphasis and one of focus that desirable extracellular timbering material is present stage organizational project.
Bone tissue engineer is a branch of organizational project.Bone tissue engineer refers to the osteoblast, bone marrow stroma stem cell or the chondrocyte that separate, after amplification in vitro is cultivated, plants in having on the timbering material of good biocompatibility; Cell is on the three-dimensional rack of prefabricated form after growing multiplication, by this cell-composite body implantable bone defect, when biomaterial is progressively degraded, the osteocyte of plantation is constantly bred, progressively form osseous tissue and bring into play corresponding function, repairing the damaged object of osseous tissue thereby reach.
Timbering material acting as in Tissue Engineering Study: for tissue or organ external structure provide the three-dimensional rack of Growth of Cells, make cell form suitable spatial distribution and the conduction of intercellular signal and interact; Special growth and differentiation signal being provided, maintaining the directed differentiation of cell, is the key of Tissue Engineering Study and clinical practice thereof.Desirable tissue engineering bracket material should have following characteristics: (1) avirulence and there is good biological tissue's compatibility, and timbering material body and catabolite thereof all can not cause the immunological rejection of body; (2) structure that has a high porosity is supported the generation with attaching, propagation and the extracellular matrix of inducing cell; (3) there is biodegradability, and degradation rate is controlled; (4) suitable plasticity and mechanical strength, to maintain the stable of timbering material microenvironment.
At present bone tissue engineering stent material mainly contains three classes: first natural biological derived material, thering is source abundant, and simple for production, histocompatibility is good and have advantages of certain biological degradability.It two is synthetic materials, as Ca-P ceramic, bioactivity glass etc.It three is composite, as inorganic macromolecular composite material, metal-polymer composite etc.Bioceramic is with its good biocompatibility and osteoinductive, have good mechanical performance and plasticity concurrently simultaneously, the requirement of bone tissue engineer to aspects such as timbering material shaping, mechanical property and osteoinductives be can meet, larger concern and application in bone tissue engineer, have been subject to.
Although multiple biologic bracket material has been carried out to many research at present, all technical barriers that biologic bracket material exists are not if cell attachment, mechanical strength etc. be still just before good solution.Especially in bone tissue engineer, the mechanical strength of timbering material often becomes the key factor of its application of restriction.Porous bioceramic scaffold generally lacks enough intensity at present, the comprcssive strength of hydroxyapatite porous bioceramic scaffold is generally no more than 10MPa, the comprcssive strength of tricalcium phosphate porous support is generally no more than 15MPa, also can only reach reluctantly the requirement of strength of spongy bone.
Beta-dicalcium silicate and activity glass belong to CaO-SiO together
2system, is considered to have biological activity.There are some researches show that osteoblast can normally attach growth on dicalcium silicate coating surface, and proliferation and differentiation, show that dicalcium silicate coating has good biocompatibility, thereby intend solving an above-mentioned difficult problem and using it for bone tissue engineer with beta-dicalcium silicate bioceramic scaffold.
Summary of the invention
The technical problem that quasi-solution of the present invention is determined is the deficiency that overcomes existing bone tissue engineering stent material, provide that a kind of mechanical strength is high, percent opening is high, to organism avirulence, beta-dicalcium silicate porous bioceramic scaffold that biocompatibility is good, and correspondingly provide a kind of preparation method and application of this beta-dicalcium silicate porous bioceramic scaffold.
For realizing above-mentioned target, the technical scheme that the present invention proposes is a kind of beta-dicalcium silicate porous bioceramic scaffold, and described beta-dicalcium silicate porous bioceramic scaffold is prepared from by following method.Specifically comprise the following steps:
(1) presoma template processing: the shape and size required according to product, obtain porous support template by organic foam processed.
(2) Ceramic Material preparation: Ca source and Si source, in suitable ratio proportioning, are added to suitable quantity of water and stabilizing agent simultaneously and carried out ball milling, the powder oven dry sieving for standby after ball milling.
(3) dipping hanging: take the prepared powder of step (2), add in proportion binding agent and distilled water to stir, be made into slurry.Sponge presoma prepared by step (1) is placed in slurry extrusion impregnating repeatedly, and squeezes out unnecessary slurry in sponge presoma.
(4) dry: the sample obtaining in step (3) is carried out to forced air drying.
(5) burn till: dried sample is put into sintering furnace high temperature sintering, and be incubated under firing temperature.
(6) cooling: insulation finishes immediately sample to be taken out from stove cooling.
In order better to solve the problems of the technologies described above, described presoma template is preferably polyurethane sponge.
The preferred mol ratio in described Ca source and Si source is 1:1 to 3:1, is particularly preferably the ratio of mol ratio 2:1.
Stabilizing agent used is preferably synthos, and its preferable amount is 0.5% ~ 3% of calcium carbonate and silicon dioxide mixed powder quality.
Described Ca source is preferably CaCO
3, CaO or Ca (HCO
3)
2, described Si source is preferably SiO
2, white carbon or the molten silicon of gas.
Described binding agent is preferably sodium carboxymethyl cellulose (CMC), and its consumption is preferably 2% ~ 4% of ball milling gained powder quality.
The moisture content in material with slurry be preferably 30% ~ 70%.
Described sintering furnace is preferably silicon molybdenum stove.
The temperature of described forced air drying is preferably controlled at 80 ~ 120 DEG C, is preferably 9-15 hour drying time.
Described calcining system is preferably segmentation to carry out, the programming rate difference of different temperatures section, and firing temperature is preferably controlled at 1200 DEG C ~ 1400 DEG C, and is preferable under firing temperature and is incubated 2 ~ 4 hours.
After described insulation finishes, preferably by sample immediately by stove take out and chilling.
The present invention also provides a kind of beta-dicalcium silicate bioceramic scaffold of preparing according to preceding method.
As a complete technical conceive, the invention provides the application of a kind of above-mentioned beta-dicalcium silicate porous bioceramic scaffold in bone tissue engineer, kind can be had osteoblastic beta-dicalcium silicate porous bioceramic scaffold to implant to repair or alternative body in damaged or downright bad osseous tissue.
Compared with prior art, the invention has the advantages that: the comprcssive strength of the prepared beta-dicalcium silicate porous bioceramic scaffold of (1) the present invention is 18 ~ 30MPa, met or exceeded the mechanical strength of spongy bone in human body, can be used for repairing spongy bone damage.(2) the present invention adopts template synthesis technique, has that plasticity is strong, shape of product and a controlled feature of size.(3) pass through technology controlling and process, beta-dicalcium silicate porous bioceramic scaffold inside and surface prepared by the present invention are intercommunicating pore structure, greatly improve mass exchange speed and the efficiency in support, for the propagation of cell and the reparative regeneration of tissue provide more effective and real microenvironment, cell can support inside and outside good attaching grow and breed.
Thus, beta-dicalcium silicate porous bioceramic scaffold set forth in the present invention is a kind of tissue engineering bracket material that has application prospect.
Brief description of the drawings
Fig. 1 is the microscopic appearance microphotograph of the beta-dicalcium silicate porous bioceramic scaffold that makes of the embodiment of the present invention 1.
Fig. 2 is the microphotograph after the beta-dicalcium silicate porous bioceramic scaffold repopulating cell that makes of the embodiment of the present invention; Wherein, A figure, B figure are respectively the microphotograph of cell culture after 7 days, 11 days.
Fig. 3 is the microscopic appearance microphotograph of the beta-dicalcium silicate porous bioceramic scaffold that makes of the embodiment of the present invention 2.
Fig. 4 is the microphotograph of 7 days after the beta-dicalcium silicate porous bioceramic scaffold repopulating cell prepared of the embodiment of the present invention 2.
Detailed description of the invention
Embodiment mono-
A beta-dicalcium silicate porous bioceramic scaffold of the present invention as shown in Figure 1, this beta-dicalcium silicate porous bioceramic scaffold be using porous organo polysilica ammonia ester foam as presoma through dipping hanging after sintering form.
The preparation method of beta-dicalcium silicate porous bioceramic scaffold of the present invention as shown in Figure 2, comprises the following steps:
(1) presoma template processing: the shape and size required according to product, obtain diameter by the processing of polyurethane sponge and be about 19mm, the thick cylinder porous support template that is about 10mm; Again will this template immerse in 10% NaOH solution and soak 6 hours, after this template is immersed in distilled water to soaking and washing 12 hours, and take out dry for standby.
(2) preparation of powder body: by CaCO
3and SiO
2mol ratio 2:1 proportioning is added the tricalcium phosphate (TCP) of above-mentioned powder quality 0.8% as stabilizing agent simultaneously.Ball milling adopts planetary ball mill ball milling, and drum's speed of rotation is 600r/min, and Ball-milling Time is 4.5 hours.Powder after ball milling takes out that to dry 100 mesh sieves for subsequent use immediately.
(3) dipping hanging: take the mixed powder in step (2), add the sodium carboxymethyl cellulose (CMC) of its mass fraction 2.5% as binding agent.After being uniformly mixed, adding dual distilled water to be made into moisture content is 40% slurry, stirs.Sponge presoma prepared by step (1) immerses in slurry extrusion impregnating repeatedly, flood rear taking-up and has crowdedly removed unnecessary slurry.
(4) dry: the sample obtaining in step (3) to be put into baking oven and at 90 DEG C, be dried 12 hours.
(5) burn till: dried sample is put into silicon molybdenum stove sintering can obtain beta-dicalcium silicate porous bioceramic scaffold.Calcining system segmentation is carried out, and the programming rate of different temperatures section is different and strictly control.Firing temperature is 1250 DEG C, under firing temperature, is incubated 4 hours.Concrete temperature increasing schedule is as shown in the table:
Table 1: temperature increasing schedule
(6) cooling: after insulation finishes, immediately sample to be taken out from stove, be placed in air ambient cooling.
The beta-dicalcium silicate porous bioceramic scaffold that the present embodiment makes has higher percent opening, and support is connective open-celled structure, and pore size is 300-550 μ m, and is evenly distributed, and comprcssive strength is 18 ~ 28MPa.The beta-dicalcium silicate porous bioceramic scaffold that the present embodiment is made, for cell culture experiments, is planted the growing state of the rear observation of cell of osteosarcoma cell (MG-63 cell).The existing a large amount of propagation of the SEM Image Display MG-63 cell of cell culture after 7 days, cell normally attaches (as Fig. 2 A) in support; The large area region of cultivating successive range in 11 days after-poppets all can be observed cell, and cell fully covers in support, and cell and cell contact are good, and a large amount of extracellular matrixs of emiocytosis (as Fig. 2 B), have presented good biocompatibility.
Embodiment bis-
The present embodiment adopts the preparation method of another beta-dicalcium silicate porous bioceramic scaffold of the present invention, comprises the following steps:
(1) presoma template processing: the shape and size required according to product, obtain diameter by the processing of polyurethane sponge and be about 19mm, the thick cylinder porous support template that is about 10mm; Again will this template immerse in 10% NaOH solution and soak 6 hours, after this template is immersed in distilled water to soaking and washing 12 hours, and take out dry for standby.
(2) preparation of powder body: by CaCO
3and SiO
2mol ratio 2:1 proportioning is added the tricalcium phosphate (TCP) of above-mentioned powder quality 2.2% as stabilizing agent simultaneously.It is for subsequent use that after ball milling, 100 mesh sieves were dried in taking-up immediately.
(3) dipping hanging: take the mixed powder in step (2), add the sodium carboxymethyl cellulose (CMC) of its mass fraction 3.5% as binding agent.After being uniformly mixed, adding dual distilled water to be made into moisture content is 60% slurry, stirs.Sponge presoma prepared by step (1) immerses in slurry extrusion impregnating repeatedly, flood rear taking-up and has crowdedly removed unnecessary slurry.
(4) dry: the sample obtaining in step (3) to be put into baking oven and at 110 DEG C, be dried 14 hours.
(5) burn till: dried sample is put into silicon molybdenum stove sintering can obtain beta-dicalcium silicate porous bioceramic scaffold.Calcining system segmentation is carried out, and the programming rate of different temperatures section is different and strictly control.Firing temperature is 1350 DEG C, under firing temperature, is incubated 4 hours.Concrete temperature increasing schedule is as shown in the table:
Table 1: temperature increasing schedule
(6) cooling: after insulation finishes, immediately sample to be taken out from stove, be placed in air ambient cooling.
The beta-dicalcium silicate porous bioceramic scaffold that the present embodiment makes as shown in Figure 3, has higher percent opening, and support is connective open-celled structure, and pore size is 300-550 μ m, and is evenly distributed, and comprcssive strength is 24 ~ 30MPa.The beta-dicalcium silicate porous bioceramic scaffold that the present embodiment is made, for cell culture experiments, is planted the growing state of the rear observation of cell of osteosarcoma cell (MG-63 cell).After cell is fixing, find by SEM electron microscopic observation, MG-63 cell can normally attach growth on support, the form of cell on support is normal, and cultivate cell after 7 days and occur significantly propagation, in support, can be observed cell and be successive range and cover in support, the extracellular matrix that emiocytosis is a large amount of, presents good biological activity, this support is also described thus, and not only mechanical strength is high, and has good biocompatibility.
Claims (7)
1. a preparation method for beta-dicalcium silicate porous bioceramic scaffold, is characterized in that, comprises the following steps:
(1) presoma template processing: the shape and size required according to product, obtain porous support template with the processing of polyurethane sponge foam, to in the NaOH solution of this template immersion 10%, soak 6 hours again, after this template is immersed in distilled water to soaking and washing 12 hours, and take out dry for standby;
(2) Ceramic Material preparation: be the ratio proportioning of 1:1 to 3:1 in molar ratio by Ca source and Si source, add suitable quantity of water and stabilizing agent simultaneously and carry out ball milling, the powder after ball milling is dried sieving for standby;
(3) dipping hanging: take the prepared powder of step (2), add in proportion the sodium carboxymethyl cellulose (CMC) of ball milling gained powder quality 2%～4% as binding agent, and add 30%～70% distilled water to stir, be made into slurry, sponge presoma prepared by step (1) is placed in slurry extrusion impregnating repeatedly, and squeezes out unnecessary slurry in sponge presoma;
(4) dry: the sample obtaining in step (3) is carried out to forced air drying;
(5) burn till: dried sample is put into sintering furnace high temperature sintering, calcining system segmentation is carried out, the programming rate difference of different temperatures section, and be incubated under firing temperature;
(6) cooling: insulation finishes immediately sample to be taken out from stove cooling.
2. the preparation method of beta-dicalcium silicate porous bioceramic scaffold according to claim 1, is characterized in that: stabilizing agent used is synthos.
3. the preparation method of beta-dicalcium silicate porous bioceramic scaffold according to claim 1, is characterized in that: the temperature of the forced air drying of sample is controlled at 80～120 DEG C, and be 9～15 hours drying time.
4. the preparation method of beta-dicalcium silicate porous bioceramic scaffold according to claim 1, is characterized in that: sample firing temperature is controlled at 1200 DEG C～1400 DEG C, and is incubated 2～4 hours under firing temperature.
5. the preparation method of beta-dicalcium silicate porous bioceramic scaffold according to claim 1, is characterized in that: insulation finish after immediately by taking out chilling in stove.
6. one kind according to claim 1 to the 5 beta-dicalcium silicate bioceramic scaffold that prepared by method described in any one.
7. the application in organizational project according to the beta-dicalcium silicate porous bioceramic scaffold described in claim 6, is applied to the reparation of os osseum tissue in bone tissue engineer and substitutes.
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| CN104556308B (en) * | 2014-12-12 | 2017-01-18 | 江苏省陶瓷研究所有限公司 | Preparation method of multivariate micro-electrolysis ceramic for water treatment |
| TWI566920B (en) * | 2015-10-08 | 2017-01-21 | A Method of Making Biodegradable Calcium Silicate Medical Ceramics by Three - dimensional Printing Technology | |
| CN105601318B (en) * | 2015-12-22 | 2018-11-30 | 广东省微生物研究所 | A kind of porous calcium phosphate calcium material and preparation method thereof |
| CN105712362A (en) * | 2016-04-25 | 2016-06-29 | 武汉科技大学 | Beta-dicalcium silicate and preparation method thereof |
| CN105999421A (en) * | 2016-05-21 | 2016-10-12 | 南昌航空大学 | Method for in-situ preparation of wollastonite porous biological ceramic bone repair materials by adoption of shells |
| CN107721449B (en) * | 2017-10-26 | 2020-11-24 | 上海理工大学 | Preparation method of porous dicalcium silicate bioactive ceramic scaffold |
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