CN101757683A - Medical porous alumina based ceramic composite material - Google Patents
Medical porous alumina based ceramic composite material Download PDFInfo
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- CN101757683A CN101757683A CN201010011440A CN201010011440A CN101757683A CN 101757683 A CN101757683 A CN 101757683A CN 201010011440 A CN201010011440 A CN 201010011440A CN 201010011440 A CN201010011440 A CN 201010011440A CN 101757683 A CN101757683 A CN 101757683A
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- diopside
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Abstract
The invention belongs to the field of biological ceramic materials, and relates to a medical porous alumina based ceramic composite material. Firstly, 1-8% of calcium fluoride, 90-98% of alumina and 1-5% of diopside are mixed according to the mass percentage, and then the calcium fluoride, the alumina and the diopside are milled by balls to prepare mixed powder; and then the mixed powder material is placed into a graphite mould to be molded and pressed, hot-pressed and sintered in the argon or nitrogen atmosphere, wherein the sintering temperature is 1400 DEG C, the pressuring temperature is 1320 DEG C, the sintering pressure is 30 MPa and the heat preservation and pressure maintaining are carried out for 30 minutes at the sintering temperature. The composite material not only has good mechanical property and bioactivity, but also is distributed with micropores on the surface and is more beneficial to the growth of bone tissues. Simultaneously, the composite material has low manufacture cost and better application prospect in terms of the restoration, replacement and the like of bones of the human body.
Description
Technical field:
The invention belongs to the bioceramic material field, particularly a kind of have higher mechanical property and the active medical porous alumina based ceramic composite material of good biological simultaneously.
Background technology:
Alumina ceramic material has advantages such as high hardness, wearability, thermostability and chemical stability, is one of the ceramic material the most widely of research at present.But aluminium oxide belongs to inert ceramic material, and pure alumina owing to there is not biological activity, can not form synostosis with body tissue as repair materials such as artificial jointes.At present the more bioactive ceramics of research is the hydroxylapatite ceramic material, and such material can carry out the chemical bond combination with being organized on the interface; But the pure ha brittleness of ceramics is big, frangibility, thus limited its extensive use.Artificial bone not only requires to possess high mechanical property, also requires to possess good biological activity.Application number is 200810015104.4 Chinese patent, disclose " a kind of alumina-based biologic active composite ", had biological activity and good mechanical performance preferably, but because material density is higher, be unfavorable for adhering to of osteocyte, influenced combining of embedded material and surrounding tissue.
Summary of the invention:
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of production cost low, have an active medical porous alumina based ceramic composite material of higher mechanical property and good biological simultaneously.
The present invention realizes in the following manner:
A kind of medical porous alumina based ceramic composite material is characterized in that adopting following method preparation:
1), batching: the mass percent of pressing calcium fluoride 1-8%, aluminium oxide 90-98%, diopside 1-5% is prepared raw material;
2), batch mixing: with the calcium fluoride in the step 1), aluminium oxide, diopside mixing and 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 argon or nitrogen atmosphere, 1400 ℃ of sintering temperatures, 1320 ℃ of pressed temperatures, sintering pressure 30MPa was sintering temperature heat-insulation pressure keeping 30 minutes.
The sample that sinters is cut into batten, after corase grind, correct grinding and polishing, ultrasonic cleaning is again put into the simulated body fluid for preparing respectively and is soaked, with the microstructure change and the sedimental generation of sem analysis sample surfaces, analyze OH with Fourier Transform Infrared spectrogrph (FT-IR)
-Functional group and PO
4 3-Whether functional group occurs, and whether contains Ga and P with electron probing analysis specimen surface product, determines that sample soaks the ability that the rear surface has very strong formation carbonated hydroxyapatite in simulated body fluid.
Calcium fluoride (CaF
2) be a kind of white powder, density is 3.18g/cm
3, 1360 ℃ of fusing points, 2500 ℃ of boiling points.Calcium fluoride (CaF
2) be not only a kind of important nucleator, and add an amount of F in the glass, by under proper temperature, being incubated, can generate the fluorophologopite phase, improve the mechanical property of composite.This test utilizes diopside and the relatively low character of calcium fluoride melting point, and the sintering processing that adopts hot pressed sintering and liquid-phase sintering to combine is in sintering process, because physical change and chemical reaction produce liquid phase in the base substrate.Because the main component of diopside is silicon dioxide, calcium oxide, magnesium oxide, the alumina matrix composite that adds calcium fluoride and diopside is in sintering process, aluminium oxide and silicon dioxide, calcium oxide, calcium fluoride, magnesium oxide etc. react and generate anorthite, magnesium aluminate, mullite, aluminium fluoride, calcium aluminate etc., thereby have improved the mechanical property of composite.Aluminium fluoride (AlF
3), 1040 ℃ of fusing points, 1260 ℃ of boiling points (distillation), density 2.88～3.18g/cm3.Because sintering temperature is up to 1400 ℃, therefore, the aluminium fluoride that generates in the sintering process can directly become gas and overflow, thereby forms pore in composite.By changing the addition of sintering process parameter and calcium fluoride, can control the quantity of pore.The result of calculation of thermodynamics also supports may taking place of above-mentioned chemical change.Existing test shows that fluorine (F) can not only promote the deposition of hydroxyapatite crystal, and, use CaF
2Can obtain more firm interface combination, but the too high meeting of F stops normal absorption of bone and reconstruction.Therefore, the adding of calcium fluoride wants an amount of.Diopside, aluminium oxide, with low cost, the aboundresources of calcium fluoride, by adopting diopside and calcium fluoride that alumina material is carried out modification, its biological activity and mechanical property have not only been improved, and improved the voidage of composite, satisfying the needs of clinical practice, is a kind of new method of low-cost preparation high-performance bio-medical ceramic composite.
The specific embodiment:
Provide three most preferred embodiments of the present invention below.
Embodiment one: the mass percent of calcium fluoride, aluminium oxide, diopside being pressed calcium fluoride 1%, aluminium oxide 98%, diopside 1% is prepared raw material.Adopt the alumina balls mixing and ball milling, 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, hot pressed sintering under nitrogen atmosphere, 1450 ℃ of sintering temperatures, sintering pressure 30 MPa, sintering time 1 hour is incubated 30 minutes.The Rockwell hardness (HRA) of the medical ceramic composite of alumina base that makes is 90.67, bending strength 381.3MPa, fracture toughness 4.68MPam
1/2With inside diameter slicer the sample that sinters is cut into the batten that is of a size of 3.3mm * 4.3mm * 36mm, after corase grind, correct grinding and polishing, ultrasonic cleaning again.Then, put into the simulated body fluid for preparing respectively.Sample soaked in calorstat 9 days, and the greenhouse is constant in 37 ℃.After in simulated body fluid, soaking, microstructure change and sedimental generation with the sem analysis sample surfaces, whether occur with Fourier Transform Infrared spectrogrph (FT-IR) analysis OH functional group and PO41-functional group, whether contain Ga and P with electron probing analysis specimen surface product.Test result shows: composite soaks the rear surface and has formed one deck osteoid apatite-carbonated hydroxyapatite (HCA) in simulated body fluid, the novel substance of generation all is the HAP structure.
Embodiment two: other is with embodiment one, and difference is that calcium fluoride, aluminium oxide, diopside are prepared raw material by the mass percent of calcium fluoride 4%, aluminium oxide 95%, diopside 1%.The Rockwell hardness of the alumina ceramic composite material that makes (HRA) is 90.37, bending strength 474.1MPa, fracture toughness 4.67MPam
1/2After testing, there are a large amount of pores on the surface, and the sample surfaces after soaking in simulated body fluid has a large amount of carbonated hydroxyapatite deposits to generate, and composite has good biological activity.
Embodiment three: other is with embodiment one, and difference is that calcium fluoride, aluminium oxide, diopside are prepared raw material by the mass percent of calcium fluoride 8%, aluminium oxide 90%, diopside 2%.The vickers hardness hv 17.40GPa of the alumina base biological ceramic composite material that makes, bending strength 446MPa, fracture toughness 4.66MPam
1/2After testing, there are a large amount of pores on the surface, and the sample after soaking in simulated body fluid is used sem analysis, and the deposit that the surface generates is osteoid apatite a---carbonated hydroxyapatite.
Claims (1)
1. medical porous alumina based ceramic composite material is characterized in that adopting following method preparation:
1), batching: the mass percent of pressing calcium fluoride 1-8%, aluminium oxide 90-98%, diopside 1-5% is prepared raw material;
2), batch mixing: with the calcium fluoride in the step 1), aluminium oxide, diopside mixing and 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 argon or nitrogen atmosphere, 1400 ℃ of sintering temperatures, 1320 ℃ of pressed temperatures, sintering pressure 30MPa was sintering temperature heat-insulation pressure keeping 30 minutes.
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|---|---|---|---|
| CN201010011440A CN101757683A (en) | 2010-01-14 | 2010-01-14 | Medical porous alumina based ceramic composite material |
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|---|---|---|---|
| CN201010011440A CN101757683A (en) | 2010-01-14 | 2010-01-14 | Medical porous alumina based ceramic composite material |
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| CN 201310034217 Division CN103073323A (en) | 2010-01-14 | 2010-01-14 | Method for preparing medical porous alumina based ceramic composite |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104744021A (en) * | 2015-03-31 | 2015-07-01 | 苏州维泰生物技术有限公司 | Wear-resisting aluminum oxide ceramic and preparation method thereof |
| CN105481354A (en) * | 2014-09-19 | 2016-04-13 | 山东大学 | Aluminum oxide-based biomedical ceramic composite material and preparation method therefor |
| CN105879110A (en) * | 2016-05-20 | 2016-08-24 | 杨景周 | Natural diopside mineral porous bio-ceramic bone repairing material |
| CN107872980A (en) * | 2015-06-23 | 2018-04-03 | I.陶瓷公司 | Breastbone replacement implants |
-
2010
- 2010-01-14 CN CN201010011440A patent/CN101757683A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481354A (en) * | 2014-09-19 | 2016-04-13 | 山东大学 | Aluminum oxide-based biomedical ceramic composite material and preparation method therefor |
| CN104744021A (en) * | 2015-03-31 | 2015-07-01 | 苏州维泰生物技术有限公司 | Wear-resisting aluminum oxide ceramic and preparation method thereof |
| CN107872980A (en) * | 2015-06-23 | 2018-04-03 | I.陶瓷公司 | Breastbone replacement implants |
| CN105879110A (en) * | 2016-05-20 | 2016-08-24 | 杨景周 | Natural diopside mineral porous bio-ceramic bone repairing material |
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Application publication date: 20100630 |