CN104774004A - Rare-earth-doped calcium phosphate bioactive ceramic and preparation method thereof - Google Patents
Rare-earth-doped calcium phosphate bioactive ceramic and preparation method thereof Download PDFInfo
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- CN104774004A CN104774004A CN201510146743.4A CN201510146743A CN104774004A CN 104774004 A CN104774004 A CN 104774004A CN 201510146743 A CN201510146743 A CN 201510146743A CN 104774004 A CN104774004 A CN 104774004A
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Abstract
The invention discloses a rare-earth-doped calcium phosphate bioactive ceramic and a preparation method thereof, relating to the field of biological materials. The rare-earth-doped calcium phosphate bioactive ceramic is prepared from the following components in parts by mass: 20-40 parts of tetracaicium phosphate, 20-40 parts of calcium hydrogen phosphate, 10-20 parts of yttrium oxide, 10-20 parts of samarium trichloride, 4-10 parts of nano titanium oxide, 5-10 parts of calcium oxide and 4-10 parts of zinc oxide. The preparation method comprises the following steps: (1) weighing; (2) ball milling; (3) cold-press molding; (4) high-temperature calcination; and (5) cooling. The rare-earth-doped calcium phosphate bioactive ceramic disclosed by the invention has the advantages of favorable biocompatibility and higher bioactivity, has certain mechanical properties, and is an ideal bone repair biological material.
Description
Technical field
The invention belongs to technical field of biological material, particularly the preparation method of a kind of rare earth doping phosphoric acid calcium bioactive ceramics and this biological ceramics.
Background technology
Along with the development of material science and technology, the property that biomaterial is repaired body tissue because of it, substituted and regenerate, has become one of important research direction of current biomedical sector.Biological hard tissue substitute material is use body bone, animal bone the earliest, develops into afterwards and adopts stainless steel and plastics, because stainless steel exists dissolved, corrosion and fatigue problem, and the problem that plastics existence and stability is poor and intensity is low.Therefore cause the bottleneck that biomaterial develops, the appearance of biological ceramics, improve the deficiency of existing equivalent material, because of its many advantages, therefore, biological ceramics is provided with vast potential for future development.
Calcium phosphate ceramic (CPC) is the important kind in biological active ceramic material, and what current investigation and application was maximum is hydroxyapatite (HA) and tricalcium phosphate (TCP).Calcium phosphate ceramic contains CaO and P
2o
5two kinds of compositions, be the important inorganic substance forming human body hard tissue, after implant into body, its surface, with the combination of tissue by key, reaches completely affine.
The title that rare earth element have " industrial VITAMIN ", has been widely used in multiple field.Most of rare earth element presents paramagnetism.Rare earth metal has plasticity-, is best with samarium and ytterbium.Except ytterbium, yttrium group rare-earth has higher hardness compared with cerium group rare-earth.
Rare earth is also widely used at ceramic field, not only for features pottery, high technology ceramics Material Field, rare earth element is widely used too, in view of rare earth element has good plasticity-, different doped level and application scenario are also not quite similar to the effect that rare earth element plays, in biological ceramics field, the application of rare earth element does not still reach good level, therefore, rare earth element being used for biomaterial, playing the performance that it is excellent, is one of developing direction of following rare earth element.
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 rare earth doping phosphoric acid calcium bioactive ceramics and preparation method thereof.
Technical scheme of the present invention: a kind of rare earth doping phosphoric acid calcium bioactive ceramics, is prepared from by each component of following mass fraction:
Tetracalcium phosphate 20-40 part, secondary calcium phosphate 20-40 part, yttrium oxide 10-20 part, Samarium chloride 10-20 part, nano-titanium oxide 4-10 part, calcium oxide 5-10 part and zinc oxide 4-10 part.
As preferably, the mass fraction of each component is: tetracalcium phosphate 25-36 part, secondary calcium phosphate 25-36 part, yttrium oxide 12-18 part, Samarium chloride 12-16 part, nano-titanium oxide 5-8 part, calcium oxide 6-9 part and zinc oxide 6-8 part.
As preferably, the mass fraction of each component is: tetracalcium phosphate 31 parts, secondary calcium phosphate 30 parts, yttrium oxide 16 parts, Samarium chloride 14 parts, nano-titanium oxide 7 parts, 8 parts, calcium oxide and 7 parts, zinc oxide.
A preparation method for rare earth doping phosphoric acid calcium bioactive ceramics, preparation process is as follows:
(1) weigh: accurately take each component;
(2) ball milling: each component mixed, puts into ball mill and carries out ground and mixed;
(3) coldmoulding: mixed powder is carried out coldmoulding;
(4) powder after shaping is put into mould, carry out high-temperature calcination, temperature is 1000 DEG C-1350 DEG C, pressure 400-700MPa, time 2-9h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid calcium bioactive ceramics.
As preferably, in step (4), the temperature of calcining is 1200 DEG C.
As preferably, in step (4), the pressure of calcining is 480MPa.
Beneficial effect: rare earth doping phosphoric acid calcium bioactive ceramics provided by the invention, be by rare earth doped among bioceramic material, play the performance that it is excellent.In technical scheme of the present invention, add yttrium oxide and Samarium chloride, there is hardness effect on the one hand that improve bioceramic material, on the other hand, the magnetic action that rare earth element has, calcium phosphate can be stimulated at bone engagement interface to produce the reactions such as decomposition, absorption and precipitation, realize mortise, promote the growth of bone.
Therefore, rare earth doping phosphoric acid calcium bioactive ceramics biocompatibility provided by the invention is better, and biological activity is higher, has certain mechanical property simultaneously, is a kind of ideal bone repair biomaterial.
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 rare earth doping phosphoric acid calcium bioactive ceramics, comprises each component of following mass fraction:
Tetracalcium phosphate 40 parts, secondary calcium phosphate 40 parts, yttrium oxide 20 parts, Samarium chloride 20 parts, nano-titanium oxide 10 parts, 10 parts, calcium oxide and 10 parts, zinc oxide.
Prepare rare earth doping phosphoric acid calcium bioactive ceramics according to preparation method provided by the invention, step is as follows:
(1) weigh: accurately take each component;
(2) ball milling: each component mixed, puts into ball mill and carries out ground and mixed;
(3) coldmoulding: adopted by mixed powder 60T press to suppress;
(4) powder after shaping is put into mould, carry out high-temperature calcination, temperature is 1300 DEG C, pressure 600MPa, time 4h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid calcium bioactive ceramics.
The block rare earth doping phosphoric acid calcium bioactive ceramics obtained is detected, detects the performance of biological ceramics: hardness 850HV; Compressive strength 1320MPa; Bending strength 570MPa; Toughness 16MPam
1/2.
Embodiment 2:
A kind of rare earth doping phosphoric acid calcium bioactive ceramics, comprises each component of following mass fraction:
Tetracalcium phosphate 20 parts, secondary calcium phosphate 20 parts, yttrium oxide 10 parts, Samarium chloride 10 parts, nano-titanium oxide 4 parts, 5 parts, calcium oxide and 4 parts, zinc oxide.
Prepare rare earth doping phosphoric acid calcium bioactive ceramics according to preparation method provided by the invention, step is as follows:
(1) weigh: accurately take each component;
(2) ball milling: each component mixed, puts into ball mill and carries out ground and mixed;
(3) coldmoulding: adopted by mixed powder 60T press to suppress;
(4) powder after shaping is put into mould, carry out high-temperature calcination, temperature is 1300 DEG C, pressure 600MPa, time 7h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid calcium bioactive ceramics.
The block rare earth doping phosphoric acid calcium bioactive ceramics obtained is detected, detects the performance of biological ceramics: hardness 830HV; Compressive strength 1270MPa; Bending strength 530MPa; Toughness 14MPam
1/2.
Embodiment 3:
A kind of rare earth doping phosphoric acid calcium bioactive ceramics, comprises each component of following mass fraction:
Tetracalcium phosphate 25 parts, secondary calcium phosphate 25 parts, yttrium oxide 12 parts, Samarium chloride 12 parts, nano-titanium oxide 5 parts, 6 parts, calcium oxide and 6 parts, zinc oxide.
Prepare rare earth doping phosphoric acid calcium bioactive ceramics according to preparation method provided by the invention, step is as follows:
(1) weigh: accurately take each component;
(2) ball milling: each component mixed, puts into ball mill and carries out ground and mixed;
(3) coldmoulding: adopted by mixed powder 60T press to suppress;
(4) powder after shaping is put into mould, carry out high-temperature calcination, temperature is 1200 DEG C, pressure 480MPa, time 6h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid calcium bioactive ceramics.
The block rare earth doping phosphoric acid calcium bioactive ceramics obtained is detected, detects the performance of biological ceramics: hardness 830HV; Compressive strength 1280MPa; Bending strength 540MPa; Toughness 14MPam
1/2.
Embodiment 4:
A kind of rare earth doping phosphoric acid calcium bioactive ceramics, comprises each component of following mass fraction:
Tetracalcium phosphate 36 parts, secondary calcium phosphate 36 parts, yttrium oxide 18 parts, Samarium chloride 16 parts, nano-titanium oxide 8 parts, 9 parts, calcium oxide and 8 parts, zinc oxide.
Prepare rare earth doping phosphoric acid calcium bioactive ceramics according to preparation method provided by the invention, step is as follows:
(1) weigh: accurately take each component;
(2) ball milling: each component mixed, puts into ball mill and carries out ground and mixed;
(3) coldmoulding: adopted by mixed powder 60T press to suppress;
(4) powder after shaping is put into mould, carry out high-temperature calcination, temperature is 1200 DEG C, pressure 480MPa, time 6h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid calcium bioactive ceramics.
The block rare earth doping phosphoric acid calcium bioactive ceramics obtained is detected, detects the performance of biological ceramics: hardness 840HV; Compressive strength 1300MPa; Bending strength 550MPa; Toughness 15MPam
1/2.
Embodiment 5:
A kind of rare earth doping phosphoric acid calcium bioactive ceramics, comprises each component of following mass fraction:
Tetracalcium phosphate 31 parts, secondary calcium phosphate 30 parts, yttrium oxide 16 parts, Samarium chloride 14 parts, nano-titanium oxide 7 parts, 8 parts, calcium oxide and 7 parts, zinc oxide.
Prepare rare earth doping phosphoric acid calcium bioactive ceramics according to preparation method provided by the invention, step is as follows:
(1) weigh: accurately take each component;
(2) ball milling: each component mixed, puts into ball mill and carries out ground and mixed;
(3) coldmoulding: adopted by mixed powder 60T press to suppress;
(4) powder after shaping is put into mould, carry out high-temperature calcination, temperature is 1200 DEG C, pressure 480MPa, time 5h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid calcium bioactive ceramics.
The block rare earth doping phosphoric acid calcium bioactive ceramics obtained is detected, detects the performance of biological ceramics: hardness 840HV; Compressive strength 1300MPa; Bending strength 550MPa; Toughness 15MPam
1/2.
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 (6)
1. a rare earth doping phosphoric acid calcium bioactive ceramics, is characterized in that, is prepared from by each component of following mass fraction:
Tetracalcium phosphate 20-40 part, secondary calcium phosphate 20-40 part, yttrium oxide 10-20 part, Samarium chloride 10-20 part, nano-titanium oxide 4-10 part, calcium oxide 5-10 part and zinc oxide 4-10 part.
2. rare earth doping phosphoric acid calcium bioactive ceramics according to claim 1, is characterized in that: the mass fraction of each component is: tetracalcium phosphate 25-36 part, secondary calcium phosphate 25-36 part, yttrium oxide 12-18 part, Samarium chloride 12-16 part, nano-titanium oxide 5-8 part, calcium oxide 6-9 part and zinc oxide 6-8 part.
3. rare earth doping phosphoric acid calcium bioactive ceramics according to claim 2, is characterized in that: the mass fraction of each component is: tetracalcium phosphate 31 parts, secondary calcium phosphate 30 parts, yttrium oxide 16 parts, Samarium chloride 14 parts, nano-titanium oxide 7 parts, 8 parts, calcium oxide and 7 parts, zinc oxide.
4. a preparation method for rare earth doping phosphoric acid calcium bioactive ceramics according to claim 1, it is characterized in that, preparation process is as follows:
(1) weigh: accurately take each component;
(2) ball milling: each component mixed, puts into ball mill and carries out ground and mixed;
(3) coldmoulding: mixed powder is carried out coldmoulding;
(4) powder after shaping is put into mould, carry out high-temperature calcination, temperature is 1000 DEG C-1350 DEG C, pressure 400-700MPa, time 2-9h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid calcium bioactive ceramics.
5. the preparation method of rare earth doping phosphoric acid calcium bioactive ceramics according to claim 4, is characterized in that: in step (4), the temperature of calcining is 1200 DEG C.
6. the preparation method of rare earth doping phosphoric acid calcium bioactive ceramics according to claim 4, is characterized in that: in step (4), the pressure of calcining is 480MPa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105217960A (en) * | 2015-09-30 | 2016-01-06 | 苏州蔻美新材料有限公司 | A kind of rear-earth-doped biological active glass ceramic and preparation method thereof |
| CN105967726A (en) * | 2016-05-06 | 2016-09-28 | 王泽陆 | Mesoporous HAP/zirconium oxide/lithium oxide artificial bone ceramic and preparation method thereof |
| CN109632739A (en) * | 2018-12-21 | 2019-04-16 | 武汉理工大学 | The quantitative detecting method of rare earth doping phosphoric acid calcium fluorescent nano particle in vivo |
| CN111017898A (en) * | 2019-12-26 | 2020-04-17 | 扬州大学 | Preparation method of iron-doped spherical calcium hydrophosphate |
-
2015
- 2015-03-31 CN CN201510146743.4A patent/CN104774004A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105217960A (en) * | 2015-09-30 | 2016-01-06 | 苏州蔻美新材料有限公司 | A kind of rear-earth-doped biological active glass ceramic and preparation method thereof |
| CN105217960B (en) * | 2015-09-30 | 2018-03-16 | 徐岩军 | A kind of rear-earth-doped biological active glass ceramic and preparation method thereof |
| CN105967726A (en) * | 2016-05-06 | 2016-09-28 | 王泽陆 | Mesoporous HAP/zirconium oxide/lithium oxide artificial bone ceramic and preparation method thereof |
| CN109632739A (en) * | 2018-12-21 | 2019-04-16 | 武汉理工大学 | The quantitative detecting method of rare earth doping phosphoric acid calcium fluorescent nano particle in vivo |
| CN109632739B (en) * | 2018-12-21 | 2021-03-16 | 武汉理工大学 | Quantitative detection method of rare earth doped calcium phosphate fluorescent nanoparticles in organism |
| CN111017898A (en) * | 2019-12-26 | 2020-04-17 | 扬州大学 | Preparation method of iron-doped spherical calcium hydrophosphate |
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Application publication date: 20150715 |