CN102211931A - Method for preparing natural hydroxyapatite biological ceramic by using microwave method - Google Patents
Method for preparing natural hydroxyapatite biological ceramic by using microwave method Download PDFInfo
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- CN102211931A CN102211931A CN201110050785XA CN201110050785A CN102211931A CN 102211931 A CN102211931 A CN 102211931A CN 201110050785X A CN201110050785X A CN 201110050785XA CN 201110050785 A CN201110050785 A CN 201110050785A CN 102211931 A CN102211931 A CN 102211931A
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Abstract
The invention discloses a method for preparing natural hydroxyapatite biological ceramic by using a microwave method. The method comprises the following steps: adding poval in natural hydroxyapatite, carrying out ball milling with a wet method, mixing and drying; insulating for 1-4 hours at the temperature of 450 DEG C in a high temperature furnace after molding in a mould, and then sintering with a microwave sintering furnace, wherein the sintering temperature is 1150 DEG C-1300 DEG C, the insulation time is 5-30 minutes; and cooling along with the furnace so as to obtain the natural hydroxyapatite biological ceramic. By using the method in the invention, the sintering time is greatly shortened, and simultaneously the mechanical property of the natural hydroxyapatite biological ceramic is improved.
Description
Technical field
The present invention relates to the method that a kind of microwave method prepares natural hydroxyl apatite bioceramic.
Background technology
Hydroxyapatite (HA) is a big focus of biomaterial development as the human body hard tissue replacement material.In recent years, the scientific research personnel puts into great effort in the research of HA whisker enhancing biological ceramic composite material.Owing to good biological activity and the biocompatibility of HA material itself, become the strongthener of biomaterial the best.Scholarly forecast is arranged, and biological activity HA whisker strengthens bioceramic material and will play a positive role for the development that promotes hard tissue substituting and repair materials.The pertinent data report, whole world biomaterial annual turnover has reached 12,000,000,000 dollars at present.Wherein, the human body hard tissue replacement material is about 2,300,000,000 dollars, and with annual 7% speed increment.This shows that along with the development of global aging trend, following human body hard tissue alternate material will more and more be subject to people's attention, this class bioactive ceramics of HA also will have wide researching value and market outlook.Bioceramic material has large development potentiality and researching value, and from bionic principle, its prepared composition structure is close with natural bone tissue.Very long history has been experienced in the research of HA biological ceramics, has obtained some achievements in clinical application, as excellent biological compatibility, biological activity, structure anastomose property etc.But improve intensity, the toughness of material how and how to solve interface problem in the ceramic coated process, and aspects such as mechanical property, biological property are still waiting further investigation and inquire into.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of microwave method to prepare the method for natural hydroxyl apatite bioceramic at the deficiencies in the prior art.
The present invention adopts following technical scheme:
A kind of microwave method prepares the method for natural hydroxyl apatite bioceramic, may further comprise the steps: get natural hydroxy phosphorus Calx powder, add polyvinyl alcohol to described natural hydroxy phosphorus Calx powder, adopt wet ball grinding mixing, drying; In High Temperature Furnaces Heating Apparatus, after 450 ℃, be incubated 1-4h after adopting mould molding, use microwave agglomerating furnace then, 1150 ℃-1300 ℃ of sintering temperatures; Soaking time 5-30min gets natural hydroxyl apatite bioceramic behind the furnace cooling.
Preferably, described sintering temperature is 1250 ℃.
Preferably, described soaking time is 10min.
Adopt method of the present invention, shorten sintering time greatly, improved the mechanical property of natural hydroxyl apatite bioceramic simultaneously.
Description of drawings
Fig. 1 is a process flow diagram of the present invention;
Concern between the linear shrinkage ratio of Fig. 2 for sintering temperature of the present invention and HA biological ceramics;
Fig. 3 is for concerning between sintering temperature of the present invention and the hungry density of HA biological ceramics.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1: referring to figs. 1 to Fig. 3, get natural hydroxy phosphorus Calx powder, add polyvinyl alcohol (add-on is 1%-5%, can according to the practical situation adjustment) to natural hydroxy phosphorus Calx powder, adopt wet ball grinding mixing 6h, drying.Use the mould of 40mm * 40mm * 5.6mm respectively, unidirectionally under 150MPa pressure be molded into square sample, pressurize 1min, blank behind the mould molding of 40mm * 40mm * 5.6mm is divided into the fritter blank of 4 40mm * 10mm * 5.6mm with saw blade, in High Temperature Furnaces Heating Apparatus, after 450 ℃, be incubated 1-4h, use microwave agglomerating furnace then, at 1150 ℃, 1200 ℃, 1250 ℃, 1300 ℃ insulation 5-30min, get four groups of different HA biological ceramics samples behind the furnace cooling respectively.Linear shrinkage ratio, density, bending strength, the Vickers' hardness of difference working sample, data refer table 1 is to table 4
Can get from table 1 to table 4: along with the rising of sintering temperature, the linear shrinkage ratio of HA biological ceramics, density, three-point bending resistance intensity etc. all raise earlier and afterwards descend, and reach maximum value in the time of 1250 ℃.In the time of 1250 ℃, linear shrinkage ratio is 13.84%, and density is 2.99gcm-3, and three-point bending resistance intensity is 65.73MPa.Can determine that thus optimal sintering temperature is 1250 ℃.
The relation of table 1 sintering temperature and linear shrinkage ratio
The relation of table 2 sintering temperature and density
The relation of table 3 sintering temperature and bending strength
The relation of table 4 sintering temperature and Vickers' hardness
Embodiment 2
As different from Example 1, when present embodiment microwave agglomerating furnace sintering temperature is 1250 ℃, be incubated 10min, 20min, 30min respectively, soaking time is the mechanical property optimum of three groups of HA biological ceramicss of 10min gained, so microwave method prepares the optimum sintering process of HA biological ceramics is: 1250 ℃ of sintering temperatures, soaking time 10min.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (3)
1. a microwave method prepares the method for natural hydroxyl apatite bioceramic, it is characterized in that, may further comprise the steps: get natural hydroxy phosphorus Calx powder, add polyvinyl alcohol to described natural hydroxy phosphorus Calx powder, adopt that wet ball grinding mixes, drying; In High Temperature Furnaces Heating Apparatus, after 450 ℃, be incubated 1-4h after adopting mould molding, use microwave agglomerating furnace then, 1150 ℃-1300 ℃ of sintering temperatures; Soaking time 5-30min gets natural hydroxyl apatite bioceramic behind the furnace cooling.
2. method according to claim 1 is characterized in that, described sintering temperature is 1250 ℃.
3. method according to claim 1 is characterized in that, described soaking time is 10min.
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| CN201110050785XA CN102211931A (en) | 2011-03-03 | 2011-03-03 | Method for preparing natural hydroxyapatite biological ceramic by using microwave method |
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| CN201110050785XA CN102211931A (en) | 2011-03-03 | 2011-03-03 | Method for preparing natural hydroxyapatite biological ceramic by using microwave method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588480A (en) * | 2013-11-19 | 2014-02-19 | 南昌航空大学 | Preparation method of secondary microwave sintering high-performance submicron zirconium oxide based tooth |
| CN108424139A (en) * | 2018-05-08 | 2018-08-21 | 西南交通大学 | A kind of high-compactness ceramic material and preparation method thereof |
| CN111320470A (en) * | 2020-01-21 | 2020-06-23 | 武汉理工大学 | Method for preparing hydroxyapatite ceramic by combining microwave hydrothermal method and microwave sintering method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101011602A (en) * | 2007-02-06 | 2007-08-08 | 西北工业大学 | Process for preparing porous biological ceramics supporting frame |
| CN101407414A (en) * | 2008-11-06 | 2009-04-15 | 上海交通大学 | Method for preparing calcium polyphosphate / tricalcium phosphate two-phase biological ceramic |
| CN101456751A (en) * | 2009-01-09 | 2009-06-17 | 北京理工大学 | Technique for preparing calcium orthophosphate base bioceramic by doping zinc oxide crystal whisker |
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2011
- 2011-03-03 CN CN201110050785XA patent/CN102211931A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101011602A (en) * | 2007-02-06 | 2007-08-08 | 西北工业大学 | Process for preparing porous biological ceramics supporting frame |
| CN101407414A (en) * | 2008-11-06 | 2009-04-15 | 上海交通大学 | Method for preparing calcium polyphosphate / tricalcium phosphate two-phase biological ceramic |
| CN101456751A (en) * | 2009-01-09 | 2009-06-17 | 北京理工大学 | Technique for preparing calcium orthophosphate base bioceramic by doping zinc oxide crystal whisker |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588480A (en) * | 2013-11-19 | 2014-02-19 | 南昌航空大学 | Preparation method of secondary microwave sintering high-performance submicron zirconium oxide based tooth |
| CN103588480B (en) * | 2013-11-19 | 2014-11-05 | 南昌航空大学 | Preparation method of secondary microwave sintering high-performance submicron zirconium oxide based tooth |
| CN108424139A (en) * | 2018-05-08 | 2018-08-21 | 西南交通大学 | A kind of high-compactness ceramic material and preparation method thereof |
| CN111320470A (en) * | 2020-01-21 | 2020-06-23 | 武汉理工大学 | Method for preparing hydroxyapatite ceramic by combining microwave hydrothermal method and microwave sintering method |
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Application publication date: 20111012 |