CN104446432A - Magnetic hydroxyapatite bioceramic and preparation method thereof - Google Patents
Magnetic hydroxyapatite bioceramic and preparation method thereof Download PDFInfo
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- CN104446432A CN104446432A CN201410626157.5A CN201410626157A CN104446432A CN 104446432 A CN104446432 A CN 104446432A CN 201410626157 A CN201410626157 A CN 201410626157A CN 104446432 A CN104446432 A CN 104446432A
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Abstract
The invention relates to a magnetic hydroxyapatite bioceramic and a preparation method thereof, belonging to the field of biomaterials. The magnetic hydroxyapatite bioceramic is prepared from the following components in parts by weight: 30-55 parts of hydroxyapatite, 6-10 parts of magnetic nano particles, 2-6 parts of magnesium oxide, 1-4 parts of nano titanium oxide, 1-3 parts of boron oxide and 6-20 parts of calcium oxide. The preparation method of the magnetic hydroxyapatite bioceramic comprises the following steps: (1) preparing the hydroxyapatite; (2) mixing the components: (3) cold-press molding powder; (4) calcining at a high temperature; and (5) cooling and taking out the finished product. The magnetic hydroxyapatite bioceramic provided by the invention has high mechanical strength, good toughness and good biocompatibility, is non-irritating, can not be absorbed, can be used for patching and filling alveolar cavities and defected bone, can be used in brain surgery and can be further used for preparing ossicular chain material and cosmetic plastic material.
Description
Technical field
The invention belongs to technical field of biological material, particularly the preparation method of a kind of magnetic hydroxylapatite biological ceramics and this biological ceramics.
Background technology
Biomaterial repairs body tissue, substitutes and the material of the performance such as regeneration.Because stainless steel exists dissolved, corrosion and fatigue problem, the problem that plastics existence and stability is poor and intensity is low.Bioceramic material obtains broad development, has comparatively wide prospect of the application.
Bioceramic material is divided into bio-inert ceramic materials and biological active ceramic material, hydroxyl apatite bioceramic is the one of bioactive ceramics, the structure of hydroxyapatite is similar to biological bone, and therefore, the hydroxyl apatite bioceramic of synthesis has the function identical with organism sclerous tissues.
Along with the development of nanotechnology, the nano magnetic particle in nano material receives the continuous concern of medical circle, and multiple magnetic Nano material has been applied to thermotherapy, nucleus magnetic resonance and technical field of biology now.In technical field of biology, magnetic nanoparticle, because possessing good biocompatibility and biomagnetism, using, having prospect of the application widely in variety carrier material.
Application number be 02129021.0 patent documentation " preparation method of nano-class hydroxyphosphorite/alumina bioceramics " disclose a kind of magnetic hydroxylapatite biological ceramics and preparation method thereof, key step is: (1) have employed the method deposited hydroxyl apatite of physics, the nanometer hydroxyapatite precursor of preparative chemistry metering ratio, ensure that settling is the hydroxyapatite of stoichiometric ratio, and employ mould plate technique; (2) hydroxyapatite precursor is nanoscale, adopt the nanometer hydroxyapatite precursor of the method preparative chemistry metering ratio of stirring heating, Heating temperature is 20-100 DEG C, and the concentration of calcium hydroxide suspension is 0.001-4mol/L, and the concentration of phosphoric acid is 0.001-5mol/L; (3) hydroxyapatite precursor supersound process being made concentration is 10
-5-10
-2the suspension liquid of mol/L, the method for directly being soaked by alumina formwork makes hydroxyapatite deposit in alumina formwork, namely obtains the nano-class hydroxyphosphorite/alumina bioceramics that orientation is consistent.
It can thus be appreciated that, this technical scheme provides magnetic hydroxylapatite bioceramic material to be the nano-class hydroxyphosphorite/alumina bioceramics utilizing sedimentation to prepare, the pottery of preparation take aluminum oxide as body material, nanometer hydroxyapatite is had in body material superficial deposit, make it have the dual property of aluminum oxide and nanometer hydroxyapatite, but because hydroxyapatite is only coated material, its performance mainly alumina matrix material, the composite boilogical ceramic of synthesis and sclerous tissues's structure of organism are also dissimilar, therefore using it as the equivalent material of bone, effect is not satisfactory.
Summary of the invention
The technical problem that the present invention solves: for above-mentioned deficiency, overcome the defect of prior art, the object of this invention is to provide a kind of magnetic hydroxylapatite biological ceramics and preparation method thereof.
Technical scheme of the present invention: a kind of magnetic hydroxylapatite biological ceramics, comprises each component of following mass fraction:
Hydroxyapatite 30-55 part, nano magnetic particle 6-10 part, magnesium oxide 2-6 part, nano-titanium oxide 1-4 part, boron oxide 1-3 part and calcium oxide 6-20 part;
Wherein, nano magnetic particle is super-paramagnetism nano Fe
3o
4particle or super-paramagnetism nano NiFe
2o
4particle.
As preferably, hydroxyapatite is prepared by hydrothermal method.
As preferably, in described hydroxyapatite, the ratio of Ga and P is 1:1.67.
As preferably, described nano-titanium oxide is rutile type nano titanium oxide.
A preparation method for magnetic hydroxylapatite biological ceramics, preparation process is as follows:
(1) hydroxyapatite is prepared: by CaHPO
4with CaCO
3prepare burden by the ratio 6:4 of amount of substance; Then wet ball grinding is carried out, time 20h; The slurry that ball milling is good is poured in container, adds distilled water, stir in 80-100 DEG C of constant temperature situation, after completion of the reaction, place the precipitation of hydroxyapatite thing that precipitation obtains white;
(2) above-mentioned precipitation of hydroxyapatite thing being carried out drying, then putting into grinding in ball grinder to mixing with other components;
(3) mixed powder is carried out coldmoulding;
(4) material after shaping is carried out high-temperature calcination, temperature is 1000 DEG C-1300 DEG C, pressure 1.5-4GPa, time 0.5-2h;
(5), after calcining, taking-up to be cooled, namely obtains block magnetic hydroxylapatite biological ceramics.
As preferably, in step (4), the temperature of calcining is 1100 DEG C-1250 DEG C.
As preferably, in step (4), the pressure of calcining is 2-3.5GPa.
Beneficial effect: magnetic hydroxylapatite biological ceramics provided by the invention is the feature utilizing hydroxyapatite similar to organism bone structure take hydroxyapatite as the magnetic hydroxyl apatite bioceramic of a kind of tool prepared by material of main part.
Hydroxyapatite has similar structure to organism sclerous tissues, and therefore function is identical, but the poor-performing of hydroxyapatite, especially compressive property and toughness, the present invention, by adding many oxide, balances the various performances of biological ceramics, and the magnetic nanoparticle added, impart the performance that biological ceramics is new, the biological ceramics synthesized thus, not only biocompatibility is better, and passes through magnetic action, can bring out new sclerous tissues's growth, effect is ideal.
Therefore, magnetic hydroxylapatite biological ceramics provided by the invention, physical strength is higher, toughness is better, there is good biocompatibility, non-stimulated, and do not absorbed, can be used for the repairing, filling etc. of alveolus, Cranial defect, cerebral surgery operation, also can be used for the material manufacturing ear auditory ossicular chain and shaping lift face.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
Embodiment 1:
A kind of magnetic hydroxylapatite biological ceramics, comprises each component of following mass fraction:
Hydroxyapatite 30 parts, super-paramagnetism nano Fe
3o
4particle 6 parts, 2 parts, magnesium oxide, rutile type nano titanium oxide 1 part, boron oxide 1 part and 6 parts, calcium oxide;
Wherein, in hydroxyapatite, the ratio of Ga and P is 1:1.67.
A preparation method for magnetic hydroxylapatite biological ceramics, preparation process is as follows:
(1) hydroxyapatite is prepared: by CaHPO
4with CaCO
3prepare burden by the ratio 6:4 of amount of substance; Then wet ball grinding is carried out, time 20h; The slurry that ball milling is good is poured in container, adds distilled water, stir in 90 DEG C of constant temperature situations, after completion of the reaction, place the precipitation of hydroxyapatite thing that precipitation obtains white;
(2) above-mentioned precipitation of hydroxyapatite thing being carried out drying, then putting into grinding in ball grinder to mixing with other components;
(3) mixed powder is carried out coldmoulding;
(4) material after shaping is carried out high-temperature calcination, temperature is 1150 DEG C, pressure 2.5 GPa, time 1h;
(5), after calcining, taking-up to be cooled, namely obtains block magnetic hydroxylapatite biological ceramics.
Performance Detection is carried out to the block magnetic hydroxylapatite biological ceramics obtained: density 3.16kg/m3; Ultimate compression strength 320MPa; Toughness 10MPam
1/2; Young's modulus 22GPa.
Embodiment 2:
A kind of magnetic hydroxylapatite biological ceramics, comprises each component of following mass fraction:
Hydroxyapatite 55 parts, super-paramagnetism nano Fe
3o
4particle 10 parts, 6 parts, magnesium oxide, rutile type nano titanium oxide 4 parts, boron oxide 3 parts and 20 parts, calcium oxide;
Wherein, in hydroxyapatite, the ratio of Ga and P is 1:1.67.
A preparation method for magnetic hydroxylapatite biological ceramics, preparation process is as follows:
(1) hydroxyapatite is prepared: by CaHPO
4with CaCO
3prepare burden by the ratio 6:4 of amount of substance; Then wet ball grinding is carried out, time 20h; The slurry that ball milling is good is poured in container, adds distilled water, stir in 90 DEG C of constant temperature situations, after completion of the reaction, place the precipitation of hydroxyapatite thing that precipitation obtains white;
(2) above-mentioned precipitation of hydroxyapatite thing being carried out drying, then putting into grinding in ball grinder to mixing with other components;
(3) mixed powder is carried out coldmoulding;
(4) material after shaping is carried out high-temperature calcination, temperature is 1200 DEG C, pressure 2.5 GPa, time 1h;
(5), after calcining, taking-up to be cooled, namely obtains block magnetic hydroxylapatite biological ceramics.
Performance Detection is carried out to the block magnetic hydroxylapatite biological ceramics obtained: density 3.15kg/m3; Ultimate compression strength 340MPa; Toughness 11MPam
1/2; Young's modulus 19GPa.
Embodiment 3:
A kind of magnetic hydroxylapatite biological ceramics, comprises each component of following mass fraction:
Hydroxyapatite 42 parts, super-paramagnetism nano NiFe
2o
4particle 8 parts, 4 parts, magnesium oxide, rutile type nano titanium oxide 2 parts, boron oxide 2 parts and 14 parts, calcium oxide;
Wherein, in hydroxyapatite, the ratio of Ga and P is 1:1.67.
A preparation method for magnetic hydroxylapatite biological ceramics, preparation process is as follows:
(1) hydroxyapatite is prepared: by CaHPO
4with CaCO
3prepare burden by the ratio 6:4 of amount of substance; Then wet ball grinding is carried out, time 20h; The slurry that ball milling is good is poured in container, adds distilled water, stir in 90 DEG C of constant temperature situations, after completion of the reaction, place the precipitation of hydroxyapatite thing that precipitation obtains white;
(2) above-mentioned precipitation of hydroxyapatite thing being carried out drying, then putting into grinding in ball grinder to mixing with other components;
(3) mixed powder is carried out coldmoulding;
(4) material after shaping is carried out high-temperature calcination, temperature is 1200 DEG C, pressure 4GPa, time 0.5h;
(5), after calcining, taking-up to be cooled, namely obtains block magnetic hydroxylapatite biological ceramics.
Performance Detection is carried out to the block magnetic hydroxylapatite biological ceramics obtained: density 3.14kg/m3; Pressure resistance 270MPa; Toughness 11MPam
1/2; Young's modulus 20GPa.
Embodiment 4:
A kind of magnetic hydroxylapatite biological ceramics, comprises each component of following mass fraction:
Hydroxyapatite 50 parts, super-paramagnetism nano NiFe
2o
4particle 7 parts, 4 parts, magnesium oxide, rutile type nano titanium oxide 3 parts, boron oxide 2 parts and 15 parts, calcium oxide;
Wherein, in hydroxyapatite, the ratio of Ga and P is 1:1.67.
A preparation method for magnetic hydroxylapatite biological ceramics, preparation process is as follows:
(1) hydroxyapatite is prepared: by CaHPO
4with CaCO
3prepare burden by the ratio 6:4 of amount of substance; Then wet ball grinding is carried out, time 20h; The slurry that ball milling is good is poured in container, adds distilled water, stir in 90 DEG C of constant temperature situations, after completion of the reaction, place the precipitation of hydroxyapatite thing that precipitation obtains white;
(2) above-mentioned precipitation of hydroxyapatite thing being carried out drying, then putting into grinding in ball grinder to mixing with other components;
(3) mixed powder is carried out coldmoulding;
(4) material after shaping is carried out high-temperature calcination, temperature is 1200 DEG C, pressure 3.5GPa, time 2h;
(5), after calcining, taking-up to be cooled, namely obtains block magnetic hydroxylapatite biological ceramics.
Performance Detection is carried out to the block magnetic hydroxylapatite biological ceramics obtained: density 3.16kg/m3; Ultimate compression strength 350MPa; Toughness 14MPam
1/2; Young's modulus 20GPa.
Embodiment 5:
A kind of magnetic hydroxylapatite biological ceramics, comprises each component of following mass fraction:
Hydroxyapatite 45 parts, super-paramagnetism nano Fe
3o
4particle 9 parts, 5 parts, magnesium oxide, rutile type nano titanium oxide 2 parts, boron oxide 2 parts and 12 parts, calcium oxide;
Wherein, in hydroxyapatite, the ratio of Ga and P is 1:1.67.
A preparation method for magnetic hydroxylapatite biological ceramics, preparation process is as follows:
(1) hydroxyapatite is prepared: by CaHPO
4with CaCO
3prepare burden by the ratio 6:4 of amount of substance; Then wet ball grinding is carried out, time 20h; The slurry that ball milling is good is poured in container, adds distilled water, stir in 90 DEG C of constant temperature situations, after completion of the reaction, place the precipitation of hydroxyapatite thing that precipitation obtains white;
(2) above-mentioned precipitation of hydroxyapatite thing being carried out drying, then putting into grinding in ball grinder to mixing with other components;
(3) mixed powder is carried out coldmoulding;
(4) material after shaping is carried out high-temperature calcination, temperature is 1250 DEG C, pressure 3GPa, time 1.5h;
(5), after calcining, taking-up to be cooled, namely obtains block magnetic hydroxylapatite biological ceramics.
Performance Detection is carried out to the block magnetic hydroxylapatite biological ceramics obtained: density 3.15kg/m3; Ultimate compression strength 330MPa; Toughness 12MPam
1/2; Young's modulus 18GPa.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (7)
1. a magnetic hydroxylapatite biological ceramics, is characterized in that, comprises each component of following mass fraction:
Hydroxyapatite 30-55 part, nano magnetic particle 6-10 part, magnesium oxide 2-6 part, nano-titanium oxide 1-4 part, boron oxide 1-3 part and calcium oxide 6-20 part;
Wherein, nano magnetic particle is super-paramagnetism nano Fe
3o
4particle or super-paramagnetism nano NiFe
2o
4particle.
2. magnetic hydroxylapatite biological ceramics according to claim 1, is characterized in that: hydroxyapatite is prepared by hydrothermal method.
3. magnetic hydroxylapatite biological ceramics according to claim 2, is characterized in that: in described hydroxyapatite, the ratio of Ga and P is 1:1.67.
4. magnetic hydroxylapatite biological ceramics according to claim 1, is characterized in that: described nano-titanium oxide is rutile type nano titanium oxide.
5. a preparation method for magnetic hydroxylapatite biological ceramics according to claim 1, it is characterized in that, preparation process is as follows:
(1) hydroxyapatite is prepared: by CaHPO
4with CaCO
3prepare burden by the ratio 6:4 of amount of substance; Then wet ball grinding is carried out, time 20h; The slurry that ball milling is good is poured in container, adds distilled water, stir in 80-100 DEG C of constant temperature situation, after completion of the reaction, place the precipitation of hydroxyapatite thing that precipitation obtains white;
(2) above-mentioned precipitation of hydroxyapatite thing being carried out drying, then putting into grinding in ball grinder to mixing with other components;
(3) mixed powder is carried out coldmoulding;
(4) material after shaping is carried out high-temperature calcination, temperature is 1000 DEG C-1300 DEG C, pressure 1.5-4GPa, time 0.5-2h;
(5), after calcining, taking-up to be cooled, namely obtains block magnetic hydroxylapatite biological ceramics.
6. the preparation method of magnetic hydroxylapatite biological ceramics according to claim 5, is characterized in that: in step (4), the temperature of calcining is 1100 DEG C-1250 DEG C.
7. the preparation method of magnetic hydroxylapatite biological ceramics according to claim 5, is characterized in that: in step (4), the pressure of calcining is 2-3.5GPa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104803674A (en) * | 2015-03-31 | 2015-07-29 | 苏州维泰生物技术有限公司 | Calcium phosphate iron bioceramic and preparation method thereof |
| CN104803672A (en) * | 2015-03-31 | 2015-07-29 | 苏州维泰生物技术有限公司 | Calcium phosphate bioactive ceramic and preparation method thereof |
| CN105274416A (en) * | 2015-09-30 | 2016-01-27 | 苏州蔻美新材料有限公司 | Magnetic zirconia biological ceramic and preparation method thereof |
| CN105837245A (en) * | 2016-03-31 | 2016-08-10 | 青岛百瑞吉生物工程有限公司 | Preparation method for hydroxyapatite porous bioceramic |
| CN106474540A (en) * | 2015-03-31 | 2017-03-08 | 陈国栋 | The bone repair preparation method of hydroxyapatite/Ti acid sodium composite boilogical ceramic |
| CN106747400A (en) * | 2016-11-22 | 2017-05-31 | 俞潮军 | A kind of high-performance bioceramic material |
| CN110408087A (en) * | 2019-08-05 | 2019-11-05 | 中国科学技术大学 | A biomimetic ceramic-based material based on nanoscale residual strain optimization and its preparation method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104803674A (en) * | 2015-03-31 | 2015-07-29 | 苏州维泰生物技术有限公司 | Calcium phosphate iron bioceramic and preparation method thereof |
| CN104803672A (en) * | 2015-03-31 | 2015-07-29 | 苏州维泰生物技术有限公司 | Calcium phosphate bioactive ceramic and preparation method thereof |
| CN106474540A (en) * | 2015-03-31 | 2017-03-08 | 陈国栋 | The bone repair preparation method of hydroxyapatite/Ti acid sodium composite boilogical ceramic |
| CN106630997A (en) * | 2015-03-31 | 2017-05-10 | 陈国栋 | Preparation method of composite biological ceramic for bone repair |
| CN105274416A (en) * | 2015-09-30 | 2016-01-27 | 苏州蔻美新材料有限公司 | Magnetic zirconia biological ceramic and preparation method thereof |
| CN105837245A (en) * | 2016-03-31 | 2016-08-10 | 青岛百瑞吉生物工程有限公司 | Preparation method for hydroxyapatite porous bioceramic |
| CN106747400A (en) * | 2016-11-22 | 2017-05-31 | 俞潮军 | A kind of high-performance bioceramic material |
| CN110408087A (en) * | 2019-08-05 | 2019-11-05 | 中国科学技术大学 | A biomimetic ceramic-based material based on nanoscale residual strain optimization and its preparation method |
| CN110408087B (en) * | 2019-08-05 | 2021-03-09 | 中国科学技术大学 | A biomimetic ceramic-based material based on nanoscale residual strain optimization and its preparation method |
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