CN1305801C - Application of magnesium olivine ceramic material as biological mechanical material - Google Patents
Application of magnesium olivine ceramic material as biological mechanical material Download PDFInfo
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- CN1305801C CN1305801C CNB2005100275359A CN200510027535A CN1305801C CN 1305801 C CN1305801 C CN 1305801C CN B2005100275359 A CNB2005100275359 A CN B2005100275359A CN 200510027535 A CN200510027535 A CN 200510027535A CN 1305801 C CN1305801 C CN 1305801C
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Abstract
The present invention relates to the application of forsterite ceramics material as biomechanics material, which is characterized in that magnesium nitrate and silicon sol are taken as the raw material, and forsterite (Mg2SiO4) powder with high purity is synthesized by adopting a sol-gel method. The synthesized powder is formed and sintered at a temperature of 1350 to 1450DEG C to obtain the forsterite ceramics. The sintered forsterite ceramics has good mechanical property, the bending strength reaches 203.4MPa, and the fracture toughness reaches 2.4MPam<1/2>, wherein the bending strength is higher than that of sintered hydroxyapatite and the compact bone of human bodies, and the fracture toughness is higher than the sintered hydroxyapatite and is close to that of the compact bone of human bodies. The prepared forsterite ceramics has good cell compatibility, supports the osteoblast anchorage and promotes the osteoblast proliferation, and therefore, the forsterite ceramics is potential bioceramics, and can serve as hard tissues repairing and implanting material.
Description
Technical field
The present invention relates to of the application of forsterite ceramics material, comprise forsterite (Mg as the biomechanics material
2SiO
4) preparation of stupalith and external biological consistency estimate, and belongs to technical field of biological material.
Background technology
Bone is damaged to be one of common clinically disease, and the reparation that bone is damaged remains insoluble clinically problem.In numerous biomaterials, biological ceramics is owing to cheap and easy to get and excellent biological compatibility become one of ideal repair materials.The more calcium phosphorus kind biological ceramics of research has excellent biological compatibility at present, yet has limited its application clinically owing to its mechanical property is relatively poor.Therefore, the new bio pottery of research and development excellent property has great importance.Studies show that in recent years, silicon ion can induced osteogenesis cell proliferations, differentiation and correlative protein expression (Bioceramics, 1998,11:265-268).Magnesium ion is one of necessary trace element of human body, and an amount of magnesium can promote osteoblastic breeding, and the direct regulation and control bone metabolism (Biomaterials, 2003,24:1389-1398).Forsterite (Mg
2SiO
1) be a kind of important compound in the silicate systems, and existing extensive studies and application in fields such as refractory materials and high frequency sound-proof materials (J.Am.Ceram.Soc, 1999,82:22-26).Protobastite (the MgSiO that has reported
3) pottery be found and have excellent mechanical property and excellent biological compatibility (Biomaterials, 1999,20:1841-1849), can be used as tooth section packing material (J.Eur.Ceram.Soc, 1998,18:2045-2056).Forsterite has the chemical constitution similar to it, also may have good mechanical performance and biocompatibility.Thereby be guided out the applicant's inventive concept.
Summary of the invention
The object of the present invention is to provide with of the application of forsterite ceramics material as the biomechanics material, specifically be to synthesize the high forsterite powder of purity by sol-gel method, and sinter forsterite ceramics at a certain temperature into, by the mechanical property to pottery, the evaluation of performances such as external scleroblast consistency determines whether it can be used as novel biological ceramics embedded material then.
Embodiment of the present invention comprises:
1. as the forsterite powder of biomechanics material application and the preparation process of pottery:
(1) silicon sol is after 1-2 stirs, at room temperature to add magnesium nitrate hexahydrate or magnesium hydroxide as the magnesium source as the Si source with the nitre acid for adjusting pH value, and the mol ratio of Mg and Si is 2: 1, stirs into homogeneous solution;
(2) mixing solutions that adds citric acid and ethylene glycol dropwise joins restir, sealing in the resultant siliceous and magnesium solution of step a; Adding mass percent is the 30-45% of synthetic forsterite powder quality;
(3) solution of step b gained, at 60 ℃ of ageing 24-48 hours, and in 120 ℃ dry 36-56 hour, make it gelation;
(4) step c gained gelation material through ball milling, sieve, 1150-1250 ℃ the calcining 3 hours, obtain pure forsterite powder;
(5) ball mill pulverizing, the dry-pressing formed hot and cold again isostatic pressing of elder generation, dry-pressing pressure 10-20MPa, waiting static pressure is 100MPa;
(6) briquetting after the last moulding was made at 1350-1450 ℃ of sintering 6-8 hour.
The weight ratio of citric acid and ethylene glycol is 3: 2 in the mixing solutions of described citric acid and ethylene glycol.
Stirring is 30 minutes during the pH value of regulating silicon sol with nitric acid in the described step (1); Add solution stirring 3-5 hour behind citric acid and the ethylene glycol in the step (2).
The particle diameter of the resultant powder of described step (5) ball milling is less than 50 microns.
Add the PVA aqueous solution of 6-10% during described moulding as binding agent.
2. the performance evaluation of the magnesium olive pottery of using as the biomechanics material
2.1 the mechanical property of pottery
Adopt the bending strength of multi-functional mechanical test machine to pottery, fracture toughness property detects.The result shows that its bending strength reaches 203.4MPa, and fracture toughness property reaches 2.4MPa m
1/2Its bending strength is higher than agglomerating hydroxyapatite (115-200MPa) and human body dense bone (50-150MPa), and fracture toughness property is higher than agglomerating hydroxyapatite (0.6-1.0MPa m
1/2) and near human body dense bone (2-12MPa m
1/2).
2.2 the biocompatibility of pottery
Adopt scleroblast to be planted on the ceramic plate, after 4 hours and 24 hours under opticmicroscope the ability of sticking of observation of cell.Electron microscope is observed osteoblastic microtexture down, through 1,3 and 7 day cultivation, adopts MTT (dimethylthiazole phenylbenzene Thiazolyl blue tetrazolium bromide salt) colorimetry to detect the multiplication capacity of cell.The result shows that scleroblast can well stick and breeds at material surface.And through 7 days cultivation, scleroblast apparently higher than blank group (p＜0.05), illustrated that forsterite ceramics has good cell compatibility at the proliferation rate on forsterite ceramics surface.(seeing description of drawings and embodiment for details)
This shows that the bending strength of the forsterite ceramics that the present invention prepares is higher than agglomerating hydroxyapatite and human body dense bone, fracture toughness property is higher than the agglomerating hydroxylapatite ceramic and near the human body dense bone.Therefore forsterite ceramics has good mechanical performance and cell in vitro consistency, is a kind of potential biological implantation material and as hard tissue repairing material.
In sum, the forsterite of biomaterial provided by the invention has good cell compatibility, supports osteoblastic adherent and stimulating osteoblast propagation, can be used as hard tissue repairing material and embedded material.
Description of drawings
By following in conjunction with the accompanying drawings the present invention being described in further details, can understand content mentioned above better.Wherein be the result of example 1 to accompanying drawing.
Fig. 1 is a sol-gel method synthetic forsterite powder XRD figure, as can be seen from the figure has only the forsterite characteristic peak to exist, and does not have other impurity.
Fig. 2 is the XRD figure of magnesium olive pottery.Forsterite ceramics after burning till does not have impurity and second to produce mutually.
Fig. 3 is magnesium olive pottery SEM figure, finds out among the figure that the forsterite ceramics surface is comparatively coarse, and this coarse surface helps sticking of cell.
Fig. 4 is that scleroblast is cultivated 4 (a) and the opticmicroscope figure after 24 (b) hours on the forsterite ceramics surface.Show the variation with incubation time among the figure, scleroblast presents significant morphological differences at material surface, for typical from being attached to the process of sprawling.
Fig. 5 cultivates 1 (a) for scleroblast on forsterite ceramics, 3 (b), 5 (c), 7 (d) days opticmicroscope figure.
Fig. 6 is the SEM figure of scleroblast after cultivating 1 day on the forsterite ceramics.From figure, be shown as osteocyte and take place to combine closely, and stretch out thread pseudopodium with material, the scleroblast smooth surface, the figure is full.
Fig. 7 is the propagation situation of scleroblast after the forsterite ceramics surface is cultivated 1,3,7 days.The result be shown as osteocyte at the rate of propagation on forsterite surface apparently higher than blank, in the time of 7 days, present significant difference (p＜0.05), the growth that forsterite ceramics can stimulating osteoblast is described.
Embodiment
The invention will be further described below in conjunction with example, but they are not that the present invention is imposed any restrictions.
Example 1:
A) silicon sol 47.06g, and add salpeter solution, regulating the pH value is 1.8, at room temperature fully stirred 30 minutes, and added 0.4 mole of magnesium nitrate hexahydrate then and stirred 3 hours, the mixture of citric acid (5.9g) and ethylene glycol (3.9g) is added drop-wise in the above-mentioned mixed solution, sealing, ageing is 48 hours in 60 ℃, and in 120 ℃ dry 36 hours, gelation.
B),, obtain pure forsterite powder, as shown in Figure 1 1200 ℃ of calcinings 3 hours with dried gel masses ball milling and sieve.
C) with synthetic forsterite powder ball milling, make its granularity after sieving, and add 6% the PVA aqueous solution less than 50 microns, earlier in the moulding of 10MPa dry-pressing forsterite powder, and under 200MPa isostatic cool pressing.
D) with the ceramic body that is pressed into 1450 ℃ of sintering 8 hours, can make forsterite ceramics, as Fig. 2, shown in 3.The surface is more coarse, helps sticking of cell.
E) forsterite ceramics of making carries out the evaluation of mechanical property and cell compatibility.Scleroblast thereon cultivation and growing state shown in Fig. 4-7, illustrate that forsterite ceramics provided by the invention is comparatively ideal as the application of biomechanics material, it has cell compatibility and has the activity that promotes Oesteoblast growth again.Shown in Figure 4, change from 4 hours to 24 hours with incubation time, scleroblast at material surface from typically being attached to the process of sprawling; Fig. 6 shows into osteocyte and takes place to combine closely with material after cultivated in 1 day on the forsterite ceramics surface, and grows thread pseudopodium, smooth surface, and the figure is full.
Example 2:
A) silicon sol 46.99g, add salpeter solution, reconciling the pH value is 1.6, at room temperature fully stirred 30 minutes, add 0.4 mole of magnesium nitrate hexahydrate then and stirred 5 hours, the mixture of citric acid (4.2g) and ethylene glycol (2.8g) is added drop-wise in the above-mentioned mixed solution, seal, ageing is 24 hours in 60 ℃, and in 120 ℃ dry 56 hours.
B) dried gel masses was calcined 3 hours at 1250 ℃, obtained pure forsterite powder.
C) with synthetic forsterite powder ball milling, make its granularity after sieving, and add 10% the PVA aqueous solution less than 60 microns, earlier in the moulding of 20MPa dry-pressing forsterite powder, and under 200MPa isostatic cool pressing.
D) with the ceramic body that is pressed into 1400 ℃ of sintering 8 hours, can make forsterite ceramics.
E) forsterite ceramics of making carries out the evaluation of mechanical property and cell compatibility, with the performance evaluation in the summary of the invention.
Its fundamental characteristics of pottery behind resulting forsterite powder and the sintering and embodiment 1 are identical.
Claims (5)
1, the forsterite ceramics material is characterized in that as the application of biomechanics material preparation process is:
(a) silicon sol is after 1-2 stirs, at room temperature to add magnesium nitrate hexahydrate or magnesium hydroxide as the magnesium source as the Si source with the nitre acid for adjusting pH value, and the mol ratio of Mg and Si is 2: 1, stirs into homogeneous solution;
(b) mixing solutions that adds citric acid and ethylene glycol dropwise joins restir, sealing in the resultant siliceous and magnesium solution of step a; Adding mass percent is the 30-45% of synthetic forsterite powder quality;
(c) solution of step b gained, at 60 ℃ of ageing 24-48 hours, and in 120 ℃ dry 36-56 hour, make it gelation;
(d) step c gained gelation material through ball milling, sieve, 1150-1250 ℃ the calcining 3 hours, obtain pure forsterite powder;
(e) ball mill pulverizing, the dry-pressing formed hot and cold again isostatic pressing of elder generation, dry-pressing pressure 10-20MPa, waiting static pressure is 100MPa;
(f) briquetting after the last moulding was made at 1350-1450 ℃ of sintering 6-8 hour.
2, by the described forsterite ceramics material of claim 1 as the application of biomechanics material, it is characterized in that the weight ratio of citric acid and ethylene glycol is 3: 2 in the mixing solutions of described citric acid and ethylene glycol.
3, by the described forsterite ceramics material of claim 1 as the application of biomechanics material, stirring is 30 minutes during the pH value that it is characterized in that regulating silicon sol with nitric acid among the described step a; Add solution stirring 3-5 hour behind citric acid and the ethylene glycol among the step b.
4, by the application of the described forsterite ceramics material of claim 1 as the biomechanics material, the particle diameter that it is characterized in that the resultant powder of described step e ball milling is less than 50 microns.
5, by the described forsterite ceramics material of claim 1 as the application of biomechanics material, add the PVA aqueous solution of 6-10% as binding agent when it is characterized in that described moulding.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100275359A CN1305801C (en) | 2005-07-01 | 2005-07-01 | Application of magnesium olivine ceramic material as biological mechanical material |
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|---|---|---|---|
| CNB2005100275359A CN1305801C (en) | 2005-07-01 | 2005-07-01 | Application of magnesium olivine ceramic material as biological mechanical material |
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|---|---|
| CN1724455A CN1724455A (en) | 2006-01-25 |
| CN1305801C true CN1305801C (en) | 2007-03-21 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102173744B (en) * | 2011-02-28 | 2013-09-11 | 吴龙华 | Ceramic dry-pressed product and preparation method thereof |
| JP6414566B2 (en) * | 2016-05-26 | 2018-10-31 | 株式会社村田製作所 | Glass-ceramic-ferrite composition and electronic component |
| CN108686716A (en) * | 2018-03-21 | 2018-10-23 | 中国科学院福建物质结构研究所 | A kind of preparation method of synthesis methyl formate carriers for catalysts |
| CN109534805B (en) * | 2018-10-16 | 2021-11-26 | 无锡顺佳特种陶瓷有限公司 | Forsterite-corundum sagger for sintering lithium battery powder and preparation method thereof |
| CN114011337B (en) * | 2021-11-09 | 2022-07-01 | 中国科学院地球化学研究所 | Preparation method of low-titanium dry forsterite single crystal under high-temperature and high-pressure conditions |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5450194A (en) * | 1977-09-27 | 1979-04-19 | Ngk Spark Plug Co | High strength portion material for living body and its preparation |
| EP0401793A1 (en) * | 1989-06-06 | 1990-12-12 | TDK Corporation | Use of ceramic materials for living hard tissue replacements |
| JP2007137853A (en) * | 2005-11-22 | 2007-06-07 | Sumitomo Chemical Co Ltd | Insect-proofing material |
-
2005
- 2005-07-01 CN CNB2005100275359A patent/CN1305801C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5450194A (en) * | 1977-09-27 | 1979-04-19 | Ngk Spark Plug Co | High strength portion material for living body and its preparation |
| EP0401793A1 (en) * | 1989-06-06 | 1990-12-12 | TDK Corporation | Use of ceramic materials for living hard tissue replacements |
| JP2007137853A (en) * | 2005-11-22 | 2007-06-07 | Sumitomo Chemical Co Ltd | Insect-proofing material |
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