CN104220102A - Porous hydroxyapatite bioceramic and preparing method thereof - Google Patents

Porous hydroxyapatite bioceramic and preparing method thereof Download PDF

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Publication number
CN104220102A
CN104220102A CN201380011760.6A CN201380011760A CN104220102A CN 104220102 A CN104220102 A CN 104220102A CN 201380011760 A CN201380011760 A CN 201380011760A CN 104220102 A CN104220102 A CN 104220102A
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porous
hydroxyapatite
lamellar
bioceramic
macropore
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CN201380011760.6A
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CN104220102B (en
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周科朝
黄智�
张斗
李志友
张妍
陈良建
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Central South University
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Central South University
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61L27/12—Phosphorus-containing materials, e.g. apatite
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61L27/50—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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61L2400/00—Materials characterised by their function or physical properties
    • A61L2400/08—Methods for forming porous structures using a negative form which is filled and then removed by pyrolysis or dissolution
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61L2430/00—Materials or treatment for tissue regeneration
    • A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants

Abstract

Disclosed are a porous hydroxyapatite bioceramic and a preparing method thereof. The porous hydroxyapatite bioceramics of the present invention has suitable pore diameters and distribution, porosity, pore-through situations, and pore surface morphology for bone tissue growth, and not only has large pores allowing a new bone to grow into, but also has abundant flake-shaped pores in pore walls, thus transferring osteogenesis. In the preparing method of the present invention, diameters and distribution of polymeric fibers are arranged appropriately in a die in advance, aqueous hydroxyapatite slurry is frozen and solidified by using orientated temperature field to make hydroxyapatite powder particulates to agglomerate and rearrange under of pushing and thrusting of an orientated grown ice crystal, a resulting ice block is frozen and dried to sublime the ice crystal before sintering is performed. The method can perform fine regulating may be performed on the porous microstructure. And porous hydroxyapatite prepared by the present invention has the high pore-through rate and the high porosity, suitable for bone tissue growth.

Description

A kind of porous hydroxyapatite bioceramic and preparation method thereof Technical field
The present invention relates to a kind of porous hydroxyapatite bioceramic and preparation method thereof.
 Background technology
The reparation of the long bone injury and defect that are caused at present by wound, inflammation and tumor resection etc. still lacks satisfied bone alternate material, as problem medically urgently to be resolved hurrily.The main restorative procedure clinically to long bone injury is that autologous bone transplanting, allograph bone, homogeneous allogenic bone transplantation and artificial bone are substituted at present.Autologous bone transplanting is treatment Cranial defect " goldstandard ", but is repairing bulk Cranial defect Shi Duigong areas tissue damage, limited for bone amount, and is also easy to produce complication, is often difficult to reach satisfied therapeutic effect.Although allograph bone and homogeneous allogenic bone transplantation avoid the infringement to being weaved for district's groups, infection rate is high, there is the danger for causing immunological rejection.Therefore, clinically all there is certain limitation in application for autologous bone and allogenic bone transplantation.Artificial synthesized bone alternate material has the advantages that easily to carry out quality control while above-mentioned unfavorable factor is avoided, also, can standardize batch production, therefore an emphasis as biomedical material research.The chemical composition and crystal structure of porous hydroxyapatite bioceramic and the inanimate matter in human body bone are similar, and with good biocompatibility, biological degradability and osteoconductive, there is very big application potential in terms of as bone tissue engineering stent material and artificial bone substitute materials.In porous calcium phosphate biological ceramic implantation bone, bone can grow into surface pore and be combined by cast setting.But internally-oriented growth of the bone tissue in hydroxyl apatite bioceramic is influenceed by factors such as the configurations of surface in the pore size of material and distribution, porosity, the insertion situation in hole and hole.There is presently no the porous hydroxyapatite bioceramic material for being well suited for bone growth.
Technical problem
It is an object of the invention to provide a kind of porous hydroxyapatite bioceramic grown into suitable for bone tissue.
 Technical solution
In order to achieve the above object, the porous hydroxyapatite bioceramic of the present invention has macropore and lamellar loose structure, wherein lamellar is porous and macropore duct angle is -45 ° ~ 45 °, macropore duct aperture is 150 ~ 1000 μm, and lamellar loose structure hole is mutually communicated with macropore duct.
Described macropore runs through whole bioceramic material.
It is preferred that, the duct interlamellar spacing of the lamellar loose structure is 10 ~ 50 μm.
It is a further object of the present invention to provide a kind of preparation method of the porous hydroxyapatite bioceramic grown into suitable for bone tissue.
In order to achieve the above object, preparation method of the invention includes：
A) will The deionized water of 95-105 parts of weight, the polyacrylamide of 0.5-2 parts of weight, the hydroxylapatite powder of the polyvinyl alcohol of 0.5-2 parts of weight and 5 ~ 150 parts of weight are well mixed, water base hydroxyapatite slurry is obtained, and is arranged with diameter for 165 ~ 1050 μm of macromolecular fibre in mould interior orientation；
b) Water base hydroxyapatite slurry is injected into mould, the low temperature directional solidification consistent with macromolecular fibre orientation is then carried out, it is 0.5 ~ 5 DEG C/min to control cooldown rate, then freezing base substrate is freezed；
C) base substrate after will be lyophilized is sintered at 1250 DEG C ~ 1350 DEG C.
Macropore duct aperture is can obtain for 150 ~ 1000 μm after c step sintering, there is the Porous Hydroxyapatite Ceramic of lamellar loose structure feature, lamellar is porous and macropore duct angle is -45 ° ~ 45 °, and lamellar loose structure hole is mutually communicated with macropore duct.
The consistent low temperature directional solidification of described macromolecular fibre orientation is the different cryogenic temperatures by controlling both mold ends so that mould inside has the temperature difference, so that ice crystal can be along macromolecular fibre orientation directional solidification growth.
It is preferred that, the macromolecular fibre is hydrophobic polymer fiber.
It is further preferred that the hydrophobic polymer fiber is terylene or nylon.
 Beneficial effect
The porous hydroxyapatite bioceramic of the present invention has the pore size and distribution, porosity, the insertion situation in hole and the configuration of surface in hole for being suitable for bone growth, not only having the macropore that can accommodate new Bone Ingrowth and being communicated with has abundant lamellar porous, so that the effect with osteoconduction.Further, since hole directional profile, ceramic mechanical property has anisotropy, there is larger compression strength along hole direction.
The preparation method of the present invention by arranging the orientation of macromolecular fibre in advance in a mold, diameter and distribution density, cryocoagulation is carried out to mould reclaimed water based hydroxylapatite slurry using thermal field is oriented, hydroxy apatite powder particle is set to carry out aggregation rearrangement in the case where the pushing of oriented growth ice crystal is repelled, by gained ice base it is freeze-dried make ice crystal distil after sinter, then leave the Porous Hydroxyapatite Ceramic with lamellar orienting stephanoporate architectural feature by template of ice, macromolecular fibre thermal cracking and volatilization in Porous Hydroxyapatite Ceramic sintering process, leave to have in Porous Hydroxyapatite Ceramic and align macropore, simultaneously, the lamellar loose structure formed in freezing casting process, it is mutually communicated ceramic inner void.By controlling the diameter of macromolecular fibre, the surface topography of polyester thread, arranging density and mode, the problem of microstructural parameters such as Porous Hydroxyapatite Ceramic pore size, pore morphology, spatial distribution are controlled is solved.Its compressive strength along hole direction can be suitable with organism dense bone.The finely regulating to porous microstructure can be achieved in the present invention, and the porous hydroxyapatite prepared with the present invention has high holing ratio of porosity and high porosity, is suitable for the growth of bone tissue.
 Brief description of the drawings
The longitudinal sectional drawing for the Porous Hydroxyapatite Ceramic that Fig. 1 is prepared for the present invention.
Fig. 2 is the porous ceramics that different big porositys are obtained by regulating and controlling the arranging density of macromolecular fibre.A：Low-density；B：Midst density；C:High density.
Fig. 3 obtains the porous ceramics with different interlamellar spacings by adjusting the weight ratio of water and hydroxyapatite powder；A：Water:Hydroxyapatite=3:2；B：Water:Hydroxyapatite=2:3.
Fig. 4 is by regulating and controlling the porosity corresponding to macromolecular fibre arranging density.None：Without macropore；low：Low-density；middle：Midst density；high：High density；Qi Zhong ▇ are that hydroxyapatite weight content is 40%, and zero is that hydroxyapatite weight content is 60%
 Embodiments of the present invention
With reference to embodiment, the invention will be further described.
Embodiment 1
1) Added into ball grinder after 100g deionized water, 1g polyacrylamides, 1g polyvinyl alcohol and 5g hydroxylapatite powders, ball milling mixing 20h, obtain water base hydroxyapatite slurry；
2) it is that 185 μm of terylene woven nets are fixed on both mold ends with diameter, then two ends mesh is each passed through with a diameter of 165 μm of polyester thread, It is allowed to arrange in mould interior orientation；
3) Water base hydroxyapatite slurry is injected after mould, progress low temperature directional solidification in the container equipped with liquid nitrogen is put into（The temperature and cooldown rate of both mold ends are controlled by controlling the flow velocity speed of both mold ends liquid nitrogen, the directional solidification of ice crystal is realized, it is as follows）, it is 5 DEG C/min to control cooldown rate, then freezes freezing base substrate in freeze drier；
4）Dried base substrate is sintered at 1350 DEG C, after sintering 1h room temperature is cooled to furnace temperature, macropore duct aperture is obtained for 150 μm, and the Porous Hydroxyapatite Ceramic with lamellar orienting stephanoporate architectural feature, wherein the duct interlamellar spacing of lamellar loose structure is 50 μm, lamellar is porous and macropore duct angle is -45 °~45 °, and lamellar loose structure hole is mutually communicated with macropore duct.
Embodiment 2
1） Added into ball grinder after 95g deionized water, 0.5g polyacrylamides, 0.5g polyvinyl alcohol and 35g hydroxylapatite powders, ball milling mixing 30h, obtain water base hydroxyapatite slurry；
2）It is that 530 μm of nylon mesh grids are fixed on both mold ends with diameter, then two ends mesh is each passed through with a diameter of 510 μm of nylon line, It is allowed to arrange in mould interior orientation；
3） Water base hydroxyapatite slurry is injected after mould, progress low temperature directional solidification in the container equipped with liquid nitrogen is put into, it is 3 DEG C/min to control cooldown rate, then freezes freezing base substrate in freeze drier；
4）Dried base substrate is sintered at 1300 DEG C, after sintering 1h room temperature is cooled to furnace temperature, macropore duct aperture is obtained for 500 μm, and the Porous Hydroxyapatite Ceramic with lamellar orienting stephanoporate architectural feature, wherein the duct interlamellar spacing of lamellar loose structure is 10 μm, lamellar is porous and macropore duct angle is -45 °~45 °, and lamellar loose structure hole is mutually communicated with macropore duct.
Embodiment 3
1）Added into ball grinder after 105g deionized water, 2g polyacrylamides, 2g polyvinyl alcohol and 150g hydroxylapatite powders, ball milling mixing 20h, obtain water base hydroxyapatite slurry；
2）It is that 1060 μm of terylene woven nets are fixed on both mold ends with diameter, then two ends mesh is each passed through with a diameter of 1050 μm of polyester thread, It is allowed to arrange in mould interior orientation；
3）Water base hydroxyapatite slurry is injected after mould, progress low temperature directional solidification in the container equipped with liquid nitrogen is put into, it is 0.5 DEG C/min to control cooldown rate, then freezes freezing base substrate in freeze drier；
4）Dried base substrate is sintered at 1250 DEG C, after sintering 1.5h room temperature is cooled to furnace temperature, macropore duct aperture is obtained for 1000 μm, and the Porous Hydroxyapatite Ceramic with lamellar orienting stephanoporate architectural feature, wherein the duct interlamellar spacing of lamellar loose structure is 40 μm, lamellar is porous and macropore duct angle is -45 °~45 °, and lamellar loose structure hole is mutually communicated with macropore duct.

Claims (7)

  1. A kind of porous hydroxyapatite bioceramic, it is characterized in that, described bioceramic has macropore and the porous structure of lamellar, wherein lamellar is porous and macropore duct angle is -45 ° ~ 45 °, macropore duct aperture is 150 ~ 1000 μm, and the porous hole of lamellar is mutually communicated with macropore duct.
  2. A kind of porous hydroxyapatite bioceramic according to claim 1, it is characterized in that, the duct interlamellar spacing of the lamellar loose structure is 10 ~ 50 μm.
  3. A kind of porous hydroxyapatite bioceramic according to claim 1, it is characterized in that, described macropore runs through whole bioceramic material.
  4. A kind of preparation method of porous hydroxyapatite bioceramic, it is characterized in that, comprise the following steps：
    A) will The deionized water of 95-105 parts of weight, the polyacrylamide of 0.5-2 parts of weight, the hydroxylapatite powder of the polyvinyl alcohol of 0.5-2 parts of weight and 5 ~ 150 parts of weight are well mixed, water base hydroxyapatite slurry is obtained, and is arranged with diameter for 165 ~ 1050 μm of macromolecular fibre in mould interior orientation；
    b) Water base hydroxyapatite slurry is injected into mould, the low temperature directional solidification consistent with macromolecular fibre orientation is then carried out, it is 0.5 ~ 5 DEG C/min to control cooldown rate, then freezing base substrate is freezed；
    C) base substrate after will be lyophilized is sintered at 1250 DEG C ~ 1350 DEG C to be obtained.
  5. Preparation method according to claim 4, it is characterized in that, macropore duct aperture is obtained after sintering for 150 ~ 1000 μm, there is the Porous Hydroxyapatite Ceramic of lamellar loose structure feature, lamellar is porous and macropore duct angle is -45 ° ~ 45 °, and lamellar loose structure hole is mutually communicated with macropore duct.
  6. A kind of preparation method of porous hydroxyapatite bioceramic according to claim 4, it is characterized in that, the macromolecular fibre is hydrophobic polymer fiber.
  7. A kind of preparation method of porous hydroxyapatite bioceramic according to claim 6, it is characterized in that, the hydrophobic polymer fiber is terylene or nylon.
CN201380011760.6A 2012-03-07 2013-03-06 A kind of porous hydroxyapatite bioceramic and preparation method thereof Active CN104220102B (en)

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PCT/CN2013/072262 WO2013131481A1 (en) 2012-03-07 2013-03-06 Porous hydroxyapatite bioceramic and preparing method thereof
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CN103588500B (en) * 2013-11-17 2014-11-05 北华航天工业学院 Preparation method of porous hydroxyapatite biological ceramic material
CN104478411B (en) * 2014-12-22 2016-09-14 成都理工大学 The method preparing high porosity growth in situ magnesium borate crystal whisker porous ceramics
CN105380732B (en) * 2015-12-14 2017-05-31 宋占涛 Bone renovating material with more-dimensional channels structure
CN105999292B (en) * 2016-05-06 2019-01-22 中南大学 A kind of preparation method of porous, hollow ceramic microballoon
CN109053183B (en) * 2018-09-03 2019-04-30 山东大学 The preparation method of bioceramic slurry for photocuring 3 D-printing
CN109157677B (en) * 2018-09-26 2021-08-31 中南大学湘雅三医院 Personalized calcium phosphate bionic bone tissue scaffold and preparation method and application thereof
CN109400200B (en) * 2018-11-30 2022-01-04 中南大学 Hydroxyapatite porous ceramic with controllable macro and micro structures and preparation method and application thereof
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