CN104220102B - A kind of porous hydroxyapatite bioceramic and preparation method thereof - Google Patents

A kind of porous hydroxyapatite bioceramic and preparation method thereof Download PDF

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CN104220102B
CN104220102B CN201380011760.6A CN201380011760A CN104220102B CN 104220102 B CN104220102 B CN 104220102B CN 201380011760 A CN201380011760 A CN 201380011760A CN 104220102 B CN104220102 B CN 104220102B
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porous
lamellar
hydroxyapatite
bioceramic
macropore
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CN104220102A (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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    • 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

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Dermatology (AREA)
  • Medicinal Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
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  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a kind of porous hydroxyapatite bioceramic and preparation method thereof.Porous hydroxyapatite bioceramic of the present invention has the pore size and distribution, porosity, the through situation in hole and the configuration of surface in hole that are suitable for bone growth, not only there is the macropore that can hold new Bone Ingrowth and hole wall has and enriches lamellar porous, thus there is the effect of osteoconduction.Preparation method of the present invention is by arranging orientation, the diameter and distribution density of macromolecular fibre in a mold in advance, directed temperature field is utilized to carry out cryocoagulation to water base hydroxyapatite slurry, make hydroxy apatite powder granule oriented growth ice crystal push repulsion under carry out gathering reset, by gained ice base sintering after lyophilization makes ice crystal distil, the finely regulating to porous microstructure can be realized, and with porous hydroxyapatite prepared by the present invention, there is high holing ratio of porosity and high porosity, be suitable for the growth of osseous tissue.

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 long bone damage caused by wound, inflammation and tumor resection etc. at present and the reparation of defect still lack satisfied bone alternate material, become a difficult problem medically urgently to be resolved hurrily.The main restorative procedure damaged long bone clinically is at present that autologous bone transplanting, allograph bone, homogeneous allogenic bone transplantation and artificial bone substitute.Autologous bone transplanting is treatment Cranial defect " goldstandard ", but at reparation bulk Cranial defect Shi Duigong district tissue damage, limited for bone amount, and easily produce complication, be often difficult to reach satisfied therapeutic effect.Although allograph bone and homogeneous allogenic bone transplantation avoid the infringement to causing for district's tissue, infection rate is high, there is the danger causing immunological rejection.Therefore, autologous bone and allogenic bone transplantation are applied clinically and all be there is certain limitation.Synthetic bone alternate material while avoiding above-mentioned unfavorable factor, also have easily carry out quality control, can the advantage such as standardization batch production, therefore become an emphasis of biomedical material research.Chemical composition and the crystal structure of the inanimate matter in porous hydroxyapatite bioceramic and human bone are similar, and there is good biocompatibility, biological degradability and bone conductibility, as in bone tissue engineering stent material and artificial bone substitute materials, there is very large application potential.In porous calcium phosphate biological ceramic implantable bone, bone can be grown into surface pore being combined by cast setting.But the autism growth of osseous tissue in hydroxyl apatite bioceramic is by the impact of the factors such as the pore size of material and distribution, porosity, the through situation in hole and the configuration of surface in hole.Also be not well suited for the porous hydroxyapatite bioceramic material of bone growth at present.
Summary of the invention
The object of this invention is to provide a kind of porous hydroxyapatite bioceramic of growing into being suitable for osseous tissue.
In order to achieve the above object, porous hydroxyapatite bioceramic of the present invention has macropore and lamellar loose structure, wherein the angle in lamellar porous and macropore duct is-45 ° ~ 45 °, aperture, macropore duct is 150 ~ 1000 μm, and lamellar loose structure hole and macropore duct mutually through.
Described macropore runs through whole bioceramic material.
Preferably, the duct interlamellar spacing of described lamellar loose structure is 10 ~ 50 μm.
Another object of the present invention is to provide a kind of preparation method being suitable for the porous hydroxyapatite bioceramic of growing into of osseous tissue.
In order to achieve the above object, preparation method of the present invention comprises:
A) by the polyacrylamide of the deionized water of 95-105 part weight, 0.5-2 part weight, the polyvinyl alcohol of 0.5-2 part weight and the hydroxylapatite powder mix homogeneously of 5 ~ 150 parts of weight, obtain water base hydroxyapatite slurry, and be that the macromolecular fibre of 165 ~ 1050 μm arranges at mould interior orientation by diameter;
B) water base hydroxyapatite slurry is injected mould, then carry out the low temperature directional solidification consistent with macromolecular fibre orientation, controlled cooling model speed is 0.5 ~ 5 DEG C/min, subsequently by freezing base substrate lyophilizing;
C) base substrate after lyophilizing is sintered at 1250 DEG C ~ 1350 DEG C.
Can obtain aperture, macropore duct after c step sintering is 150 ~ 1000 μm, there is the Porous Hydroxyapatite Ceramic of lamellar loose structure feature, the angle in lamellar porous and macropore duct is-45 ° ~ 45 °, and lamellar loose structure hole and macropore duct mutually through.
The consistent low temperature directional solidification of described macromolecular fibre orientation is the different cryogenic temperatures by controlling both mold ends, makes mould inside there is the temperature difference, thus makes ice crystal can along macromolecular fibre orientation directional solidification growth.
Preferably, described macromolecular fibre is hydrophobic polymer fiber.
Preferred further, described hydrophobic polymer fiber is terylene or nylon.
Porous hydroxyapatite bioceramic of the present invention has the pore size and distribution, porosity, the through situation in hole and the configuration of surface in hole that are suitable for bone growth, not only there is the macropore that can hold new Bone Ingrowth and be communicated with to have and enrich lamellar porous, thus there is the effect of osteoconduction.In addition, due to hole directional profile, the mechanical property of pottery has anisotropy, has larger comprcssive strength along hole direction.
Preparation method of the present invention is by arranging the orientation of macromolecular fibre in a mold in advance, diameter and distribution density, directed temperature field is utilized to carry out cryocoagulation to hydroxyapatite slurry water base in mould, make hydroxy apatite powder granule oriented growth ice crystal push repulsion under carry out gathering reset, by gained ice base sintering after lyophilization makes ice crystal distil, then staying with ice is the Porous Hydroxyapatite Ceramic with lamellar orienting stephanoporate architectural feature of template, macromolecular fibre is thermal cracking and volatilization in Porous Hydroxyapatite Ceramic sintering process, stay to have in Porous Hydroxyapatite Ceramic and align macropore, simultaneously, the lamellar loose structure formed in freezing casting process, make ceramic inner void mutually through.By controlling the diameter of macromolecular fibre, the surface topography of polyester thread, arranging density and mode, solve the problem that the microstructural parameters such as Porous Hydroxyapatite Ceramic pore size, pore morphology, spatial distribution control.Its compressive strength along direction, hole can be suitable with organism compact bone.The present invention can realize the finely regulating to porous microstructure, and has high holing ratio of porosity and high porosity with porous hydroxyapatite prepared by the present invention, is suitable for the growth of osseous tissue.
Accompanying drawing explanation
Fig. 1 is longitudinal sectional drawing of Porous Hydroxyapatite Ceramic prepared by the present invention.
Fig. 2 is the porous ceramics that the arranging density by regulating and controlling macromolecular fibre obtains different large porosity.A: low-density; B: Midst density; C: high density.
Fig. 3 obtains the porous ceramics with different layers spacing by regulating the weight ratio of water and hydroxyapatite powder; A: water: hydroxyapatite=3:2; B: water: hydroxyapatite=2:3.
Fig. 4 is by the porosity corresponding to regulation and control macromolecular fibre arranging density.None: without macropore; Low: low-density; Middle: Midst density; High: high density; Qi Zhong ▇ to be hydroxyapatite weight content be 40%, zero for hydroxyapatite weight content be 60%.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
1) in ball grinder, add the deionized water of 100g, 1g polyacrylamide, 1g polyvinyl alcohol and 5g hydroxylapatite powder, after ball milling mixing 20h, obtain water base hydroxyapatite slurry;
2) be that 185 μm of terylene woven nets are fixed on both mold ends by diameter, then be each passed through two ends mesh with the polyester thread that diameter is 165 μm, make it to arrange at mould interior orientation;
3) after water base hydroxyapatite slurry being injected mould, put into the container that liquid nitrogen is housed to carry out low temperature directional solidification (the flow velocity speed namely by controlling both mold ends liquid nitrogen controls temperature and the cooldown rate of both mold ends, realize the directional solidification of ice crystal, as follows), controlled cooling model speed is 5 DEG C/min, subsequently by the lyophilizing in freezer dryer of freezing base substrate;
4) dried base substrate is sintered at 1350 DEG C, room temperature is cooled to furnace temperature after sintering 1h, obtaining aperture, macropore duct is 150 μm, and there is the Porous Hydroxyapatite Ceramic of lamellar orienting stephanoporate architectural feature, wherein the duct interlamellar spacing of lamellar loose structure is 50 μm, the angle in lamellar porous and macropore duct is-45 ° ~ 45 °, and lamellar loose structure hole and macropore duct mutually through.
Embodiment 2
1) in ball grinder, add the deionized water of 95g, 0.5g polyacrylamide, 0.5g polyvinyl alcohol and 35g hydroxylapatite powder, after ball milling mixing 30h, obtain water base hydroxyapatite slurry;
2) be that 530 μm of nylon mesh grids are fixed on both mold ends by diameter, then be each passed through two ends mesh with the nylon line that diameter is 510 μm, make it to arrange at mould interior orientation;
3), after water base hydroxyapatite slurry being injected mould, put into the container that liquid nitrogen is housed and carry out low temperature directional solidification, controlled cooling model speed is 3 DEG C/min, subsequently by the lyophilizing in freezer dryer of freezing base substrate;
4) dried base substrate is sintered at 1300 DEG C, room temperature is cooled to furnace temperature after sintering 1h, obtaining aperture, macropore duct is 500 μm, and there is the Porous Hydroxyapatite Ceramic of lamellar orienting stephanoporate architectural feature, wherein the duct interlamellar spacing of lamellar loose structure is 10 μm, the angle in lamellar porous and macropore duct is-45 ° ~ 45 °, and lamellar loose structure hole and macropore duct mutually through.
Embodiment 3
1) in ball grinder, add the deionized water of 105g, 2g polyacrylamide, 2g polyvinyl alcohol and 150g hydroxylapatite powder, after ball milling mixing 20h, obtain water base hydroxyapatite slurry;
2) be that 1060 μm of terylene woven nets are fixed on both mold ends by diameter, then be each passed through two ends mesh with the polyester thread that diameter is 1050 μm, make it to arrange at mould interior orientation;
3), after water base hydroxyapatite slurry being injected mould, put into the container that liquid nitrogen is housed and carry out low temperature directional solidification, controlled cooling model speed is 0.5 DEG C/min, subsequently by the lyophilizing in freezer dryer of freezing base substrate;
4) dried base substrate is sintered at 1250 DEG C, room temperature is cooled to furnace temperature after sintering 1.5h, obtaining aperture, macropore duct is 1000 μm, and there is the Porous Hydroxyapatite Ceramic of lamellar orienting stephanoporate architectural feature, wherein the duct interlamellar spacing of lamellar loose structure is 40 μm, the angle in lamellar porous and macropore duct is-45 ° ~ 45 °, and lamellar loose structure hole and macropore duct mutually through.

Claims (3)

1. a preparation method for porous hydroxyapatite bioceramic, is characterized in that, comprises the following steps:
A) by the polyacrylamide of the deionized water of 95-105 part weight, 0.5-2 part weight, the polyvinyl alcohol of 0.5-2 part weight and the hydroxylapatite powder mix homogeneously of 5 ~ 150 parts of weight, obtain water base hydroxyapatite slurry, and be that the macromolecular fibre of 165 ~ 1050 μm arranges at mould interior orientation by diameter;
B) water base hydroxyapatite slurry is injected mould, then carry out the low temperature directional solidification consistent with macromolecular fibre orientation, controlled cooling model speed is 0.5 ~ 5 DEG C/min, subsequently by freezing base substrate lyophilizing; The consistent low temperature directional solidification of described macromolecular fibre orientation is the different cryogenic temperatures by controlling both mold ends, makes mould inside there is the temperature difference, thus makes ice crystal can along macromolecular fibre orientation directional solidification growth;
C) base substrate after lyophilizing is carried out sintering at 1250 DEG C ~ 1350 DEG C to obtain;
Described bioceramic has the structure of macropore and lamellar porous; Obtaining aperture, macropore duct after sintering is 150 ~ 1000 μm, has the Porous Hydroxyapatite Ceramic of lamellar loose structure feature, and the angle in lamellar porous and macropore duct is-45 ° ~ 45 °, and lamellar loose structure hole and macropore duct mutually through; Described macropore runs through whole bioceramic material; The duct interlamellar spacing of described lamellar loose structure is 10 ~ 50 μm.
2. the preparation method of a kind of porous hydroxyapatite bioceramic according to claim 1, is characterized in that, described macromolecular fibre is hydrophobic polymer fiber.
3. the preparation method of a kind of porous hydroxyapatite bioceramic according to claim 2, is characterized in that, described 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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