CN1935270A - Hydroxy apatite-base composite bioceramic material, and its preparing process - Google Patents
Hydroxy apatite-base composite bioceramic material, and its preparing process Download PDFInfo
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- CN1935270A CN1935270A CN 200610069159 CN200610069159A CN1935270A CN 1935270 A CN1935270 A CN 1935270A CN 200610069159 CN200610069159 CN 200610069159 CN 200610069159 A CN200610069159 A CN 200610069159A CN 1935270 A CN1935270 A CN 1935270A
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- hydroxyapatite
- diopside
- sintering
- aluminium oxide
- hydroxy apatite
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Abstract
The present invention relates to a composite biological ceramic material using hydroxyapatite as base body and using diopside and alumina as toughening reinforcing body. Its composition includes (by wt%) 58-89% of hydroxyapatite, 0.5-2% of diopside and 10-40% of alumina, and its preparation method includes the following steps: mixing materials, ball-grinding, hot-pressing and sintering, its sintering temperature is 1300-1320 deg.C and sintering pressure is 20-30 MPa, and its heat-insulating and pressure-holding time is 30-60 min.
Description
Technical field
The invention belongs to material science and biomedical crossing domain, particularly a kind of is that matrix, diopside and aluminium oxide are the composite bioceramic material and the preparation technology thereof of toughened and reinforced body with the hydroxylapatite ceramic material.
Background technology
Hydroxyapatite (Hydroxyapatite, HA or HAP) is the bioactive materials that a class has good biocompatibility, can be on the interface behind the implantable bone tissue and the very strong chemical bonding of bone formation, have bone conduction and osteoinductive.Yet,, thereby be limited in the non-dynamic load environment by strictness and use because the fragility height of hydroxyapatite own, rupture strength and fracture toughness are low.Therefore be restricted in the load-bearing material application facet, and it is functional not outstanding.The enhanced hydroxyapatite composite material of whisker has good toughening effect, but whisker is considered to potential carcinogen.In addition, being used for enhanced whisker can enter human body from hydroxyapatite, causes serious health problem easily.Hydroxyapatite and zirconic composite are to study a more class composite at present.The rupture strength of such material is ceramic higher than pure ha, has certain biocompatibility, but still can not surpass the human body compact bone, can only be used for some repairing aspect, and can not be used for human loaded bone.The patent No. is that 02136031.6 Chinese patent discloses a kind of " the compound method for preparing chitosan/hydroxyapatite nano composite of original position ", and the original position synthesized polymer is prepared the chitosan/hydroxyapatite nano composite of transparent little Huang.But the bending strength of material only can reach 89 ± 4MPa, and bending modulus is 3.5 ± 0.1GPa, all far below the normal parameter of human body bone.The patent No. is that another Chinese patent of 03112066.0 discloses a kind of " hydroxylapatite/carbon nanotube composite and preparation technology thereof ", and the main mechanical property of prepared material improves a lot: bending strength 90～180MPa, fracture toughness K
IC1.0～2.8MPam
1/2But the adding of CNT makes preparation cost improve greatly, and the mechanical property fluctuation range of composite is bigger.Test and also find when the CNT mass content surpasses 25%, because carbon nanotube density is less, matrix and wild phase location swap, the temperature about 1300 ℃ is difficult to synthetic material requested.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of cost low, not only have higher mechanical property but also have hydroxy apatite-base composite bioceramic material of excellent biological compatibility and preparation method thereof.
The present invention realizes in the following manner:
Hydroxy apatite-base composite bioceramic material, it is characterized in that it is that feedstock production forms by hydroxyapatite, diopside, aluminium oxide, each raw material mass percent (wt%) be: hydroxyapatite 58～89%, diopside 0.5～2%, aluminium oxide 10～40%.
The processing step for preparing above-mentioned hydroxy apatite-base composite bioceramic material is:
1), batching: the mass percent of pressing hydroxyapatite 58～89%, diopside 0.5～2%, aluminium oxide 10～40% is prepared raw material;
2), ball milling: the hydroxyapatite in the step 1), aluminium oxide, diopside are mixed, adopt the alumina balls ball milling, the powder behind the ball milling makes mixed powder by 100 mesh sieves;
3), sintering: with the compression molding in the graphite jig of packing into of mixed powder material, hot pressed sintering under nitrogen atmosphere, 20 ℃/minute of programming rates, sintering temperature 1300-1320 ℃, sintering pressure 20-30MPa, heat-insulation pressure keeping 30-60 minute.
The hydroxy apatite-base composite bioceramic material of the present invention preparation has excellent biological compatibility and than mechanical properties such as the better fracture toughness of pure HA, bending strengths, can be used for the aspect such as reparation, replacement of human body bone, in the damaged reparation of bone, good prospects for application is arranged.Diopside forms liquid phase in sintering process, can reduce the diffusion mass transfer resistance, and the mass transfer velocity that accelerate to flow for hydroxyapatite and alumina grain provide the fast transferring path, thereby can reduce sintering temperature, quickens blank Densification.Diopside, with low cost, the aboundresources of aluminium oxide have found a kind of low-cost new method for preparing the medical ceramic material of high-performance hydroxy apatite-base compound bio.
The specific embodiment
Provide two most preferred embodiments of the present invention below:
Embodiment one: the mass percent of hydroxyapatite, aluminium oxide, diopside being pressed hydroxyapatite 89.5%, aluminium oxide 10%, diopside 0.5% is prepared raw material, adopt the alumina balls mixing and ball milling, 70 hours ball milling time, the powder behind the ball milling makes mixed powder by 100 mesh sieves.With the mixed powder compression molding in the graphite jig of packing into, at the nitrogen atmosphere hot pressed sintering, 1320 ℃ of sintering temperatures, sintering pressure 28MPa, sintering time 1 hour is incubated 30 minutes.Make the vickers hardness hv 4.0GPa of hydroxy apatite-base composite bioceramic material, bending strength 103MPa, fracture toughness 2.50MPam
1/2
Embodiment two: other is with embodiment one, difference is that hydroxyapatite, aluminium oxide, diopside are prepared raw material by the mass percent of hydroxyapatite 79%, aluminium oxide 20%, diopside 1%, 1300 ℃ of sintering temperatures, sintering pressure 20MPa, be incubated 40 minutes, the vickers hardness hv 4.64GPa of the hydroxy apatite-base composite bioceramic material that makes, bending strength 128MPa, fracture toughness 2.26MPam
1/2
Embodiment three: other is with embodiment one, difference is that hydroxyapatite, aluminium oxide, diopside are prepared raw material by the mass percent of hydroxyapatite 58%, aluminium oxide 40%, diopside 2%, 1310 ℃ of sintering temperatures, sintering pressure 30MPa, be incubated 60 minutes, the vickers hardness hv 5.87GPa of the hydroxy apatite-base composite bioceramic material that makes, bending strength 200MPa, fracture toughness 2.78MPam
1/2
Claims (2)
1. hydroxy apatite-base composite bioceramic material, it is characterized in that it is that feedstock production forms by hydroxyapatite, diopside, aluminium oxide, each raw material mass percent (wt%) be: hydroxyapatite 58～89%, diopside 0.5～2%, aluminium oxide 10～40%.
2. technology for preparing the described hydroxy apatite-base composite bioceramic material of claim 1 is characterized in that may further comprise the steps:
1), batching: the mass percent of pressing hydroxyapatite 58～89%, diopside 0.5～2%, aluminium oxide 10～40% is prepared raw material;
2), ball milling: the hydroxyapatite in the step 1), aluminium oxide, diopside are mixed, adopt the alumina balls ball milling, the powder behind the ball milling makes mixed powder by 100 mesh sieves;
3), sintering: with the compression molding in the graphite jig of packing into of mixed powder material, hot pressed sintering under nitrogen atmosphere, 20 ℃/minute of programming rates, sintering temperature 1300-1320 ℃, sintering pressure 20-30MPa, heat-insulation pressure keeping 30-60 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100691594A CN100411693C (en) | 2006-10-17 | 2006-10-17 | Hydroxy apatite-base composite bioceramic material, and its preparing process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100691594A CN100411693C (en) | 2006-10-17 | 2006-10-17 | Hydroxy apatite-base composite bioceramic material, and its preparing process |
Publications (2)
| Publication Number | Publication Date |
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| CN1935270A true CN1935270A (en) | 2007-03-28 |
| CN100411693C CN100411693C (en) | 2008-08-20 |
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| CNB2006100691594A Expired - Fee Related CN100411693C (en) | 2006-10-17 | 2006-10-17 | Hydroxy apatite-base composite bioceramic material, and its preparing process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102303977A (en) * | 2011-05-24 | 2012-01-04 | 东北大学 | Method for preparing titanium-iron particle reinforced hydroxyapatite-based bioceramic material |
| CN104987058A (en) * | 2015-06-24 | 2015-10-21 | 山东大学 | Method for preparing hydroxyapatite-based composite bioceramic material through in-situ reaction |
| CN105481354A (en) * | 2014-09-19 | 2016-04-13 | 山东大学 | Aluminum oxide-based biomedical ceramic composite material and preparation method therefor |
| CN108002840A (en) * | 2017-11-30 | 2018-05-08 | 明光市裕阳新材料有限公司 | A kind of biology implantation ceramic material and preparation method |
| CN108772559A (en) * | 2018-06-15 | 2018-11-09 | 南方科技大学 | A kind of bioceramic Base Metal composite material and preparation method and purposes |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5032552A (en) * | 1988-07-04 | 1991-07-16 | Tdk Corporation | Biomedical material |
| CN1092395A (en) * | 1994-02-24 | 1994-09-21 | 朱海临 | The nine-five aluminium oxide ceramic that sintering temperature is low |
| CN1076716C (en) * | 1997-12-16 | 2001-12-26 | 武汉工业大学 | Process for mfg. non-lumps submicron alpha-Al2O3 powder and microlitic corundum ball |
| CN1397518A (en) * | 2002-08-28 | 2003-02-19 | 中国科学院长春应用化学研究所 | Process for preparing nano-class hydroxyphosphorite/alumina bioceramics |
| RU2233650C1 (en) * | 2003-05-05 | 2004-08-10 | Томский политехнический университет | Charge for preparing glass ceramic material for stomatology |
| CN1326802C (en) * | 2005-08-22 | 2007-07-18 | 山东大学 | Aluminum oxide/diopside ceramic composite material and its preparation method |
-
2006
- 2006-10-17 CN CNB2006100691594A patent/CN100411693C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102303977A (en) * | 2011-05-24 | 2012-01-04 | 东北大学 | Method for preparing titanium-iron particle reinforced hydroxyapatite-based bioceramic material |
| CN105481354A (en) * | 2014-09-19 | 2016-04-13 | 山东大学 | Aluminum oxide-based biomedical ceramic composite material and preparation method therefor |
| CN104987058A (en) * | 2015-06-24 | 2015-10-21 | 山东大学 | Method for preparing hydroxyapatite-based composite bioceramic material through in-situ reaction |
| CN104987058B (en) * | 2015-06-24 | 2017-10-17 | 山东大学 | A kind of method that reaction in-situ prepares hydroxy apatite-base composite bioceramic material |
| CN108002840A (en) * | 2017-11-30 | 2018-05-08 | 明光市裕阳新材料有限公司 | A kind of biology implantation ceramic material and preparation method |
| CN108772559A (en) * | 2018-06-15 | 2018-11-09 | 南方科技大学 | A kind of bioceramic Base Metal composite material and preparation method and purposes |
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| CN100411693C (en) | 2008-08-20 |
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Granted publication date: 20080820 Termination date: 20121017 |