CN104744024A - Rare-earth-doped tricalcium phosphate bioceramic and preparation method thereof - Google Patents

Rare-earth-doped tricalcium phosphate bioceramic and preparation method thereof Download PDF

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Publication number
CN104744024A
CN104744024A CN201510146659.2A CN201510146659A CN104744024A CN 104744024 A CN104744024 A CN 104744024A CN 201510146659 A CN201510146659 A CN 201510146659A CN 104744024 A CN104744024 A CN 104744024A
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parts
rare earth
phosphoric acid
biological ceramics
tricalcium phosphate
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殷飞
刘大学
李永超
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SUZHOU VIVOTIDE BIOTECHNOLOGIES CO Ltd
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SUZHOU VIVOTIDE BIOTECHNOLOGIES CO Ltd
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Abstract

The invention discloses a rare-earth-doped tricalcium phosphate bioceramic and a preparation method thereof, relating to the field of biological materials. The rare-earth-doped tricalcium phosphate bioceramic is prepared from the following components in parts by mass: 42-62 parts of tricalcium phosphate, 12-22 parts of praseodymium oxide, 5-10 parts of ytterbium trichloride, 3-8 parts of titanium diboride, 5-10 parts of zirconium oxide and 3-6 parts of silicon nitride. 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 tricalcium phosphate bioceramic disclosed by the invention has the advantages of favorable biocompatibility, higher bioactivity, certain anti-inflammatory and bactericidal properties and favorable mechanical properties, and can be used as a skeleton repair instead of the biological material.

Description

A kind of rare earth doping phosphoric acid DFP biological ceramics and preparation method thereof
Technical field
The invention belongs to technical field of biological material, particularly the preparation method of a kind of rare earth doping phosphoric acid DFP biological 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.
The biodegradable ceramic bata-tricalcium phosphate (being called for short β-TCP) of current widespread use, belong to trigonal system, calcium phosphorus atom ratio is 1.5, is a kind of high-temperature-phase of calcium phosphate.The sharpest edges of β-TCP are exactly good biocompatibility, directly merge after implanting to human body with bone, without any local inflammatory response and whole body toxic side effect.
Ratio of calcium and phosphorus in decision body, solvability and absorption trend plays an important role, and is easier to dissolve in vivo so compare TCP with HA, and its solubleness about than HA height 10-20 doubly.Conventional β-TCP implants and can degrade gradually, and degradation rate can because of its surface structure, crystallographic configurations, and different containing porosity and the difference implanting animal, its intensity often weakens with degraded.
With other ceramic phase ratios, β-TCP pottery is more similar to the character of people's bone and natural teeth and structure in vivo, the dissolving of hydroxyapatite is harmless, and rely on and supplement the new bone of the formation such as calcium and phosphate anion from body fluid, the reactions such as decomposition, absorption and precipitation can be produced at bone engagement interface, realize mortise.
The shortcoming of β-TCP pottery is that physical strength is on the low side, is unable to undergo the impact of power.Being mixed with other materials by β-TCP, make two-phase or multiphase ceramic, is one of method improving its mechanical strength.
The title that rare earth element have " industrial VITAMIN ", has been widely used in multiple field.Be widely used at ceramic field rare earth element, at present, rare earth promotes plant production at agriculture field, and the effect improving output is confirmed.Due to the plasticity-of rare earth, " rare earth medical treatment " occurs, also rests on the experimental phase at present, but it is to the active effect of viable cell and tissue, has obtained certainly.
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 DFP biological ceramics and preparation method thereof.
Technical scheme of the present invention: a kind of rare earth doping phosphoric acid DFP biological ceramics, is prepared from by each component of following mass fraction:
Tricalcium phosphate 42-62 part, Praseodymium trioxide 12-22 part, ytterbium trichloride 5-10 part, TiB2 3-8 part, zirconium white 5-10 part and silicon nitride 3-6 part.
As preferably, the mass fraction of each component is: tricalcium phosphate 48-56 part, Praseodymium trioxide 14-18 part, ytterbium trichloride 6-8 part, TiB2 5-8 part, zirconium white 6-9 part and silicon nitride 4-5 part.
As preferably, the mass fraction of each component is: tricalcium phosphate 54 parts, Praseodymium trioxide 17 parts, ytterbium trichloride 7 parts, TiB2 6 parts, zirconium white 8 parts and silicon nitride 4 parts.
A preparation method for rare earth doping phosphoric acid DFP biological 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 1100 DEG C-1500 DEG C, pressure 400-800MPa, time 3-10h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid DFP biological ceramics.
As preferably, in step (4), the temperature of calcining is 1380 DEG C.
As preferably, in step (4), the pressure of calcining is 650MPa.
Beneficial effect: rare earth doping phosphoric acid DFP biological 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 Praseodymium trioxide and ytterbium trichloride, both all can improve the mechanical property of bioceramic material on the one hand, on the other hand, biological ceramics can be made to possess the performance of certain anti-inflammatory sterilization, time in implant into body, have certain sterilization anti-inflammatory action, and, rare earth can irritation cell, and excites osseous tissue from body fluid, supplement calcium and phosphate anion etc. to form new bone, realize and bioactive ceramics mortise.
Therefore, rare earth doping phosphoric acid DFP biological ceramics biocompatibility provided by the invention is better, and biological activity is higher, has certain anti-inflammatory bactericidal property, meanwhile, possesses good mechanical property, can be used as bone repair and substitute 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 DFP biological ceramics, comprises each component of following mass fraction:
Tricalcium phosphate 62 parts, Praseodymium trioxide 22 parts, ytterbium trichloride 10 parts, TiB2 8 parts, zirconium white 10 parts and silicon nitride 6 parts.
Prepare rare earth doping phosphoric acid DFP biological 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 1450 DEG C, pressure 700MPa, time 4h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid DFP biological ceramics.
The block rare earth doping phosphoric acid DFP biological ceramics obtained is tested, detects the performance of biological ceramics: hardness 950HV; Compressive strength 1660MPa; Bending strength 680MPa; Toughness 17MPam 1/2.
Embodiment 2:
A kind of rare earth doping phosphoric acid DFP biological ceramics, comprises each component of following mass fraction:
Tricalcium phosphate 42 parts, Praseodymium trioxide 12 parts, ytterbium trichloride 5 parts, TiB2 3 parts, zirconium white 5 parts and silicon nitride 3 parts.
Prepare rare earth doping phosphoric acid DFP biological 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 1450 DEG C, pressure 500MPa, time 7h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid DFP biological ceramics.
The block rare earth doping phosphoric acid DFP biological ceramics obtained is tested, detects the performance of biological ceramics: hardness 920HV; Compressive strength 1610MPa; Bending strength 640MPa; Toughness 15MPam 1/2.
Embodiment 3:
A kind of rare earth doping phosphoric acid DFP biological ceramics, comprises each component of following mass fraction:
Tricalcium phosphate 56 parts, Praseodymium trioxide 18 parts, ytterbium trichloride 8 parts, TiB2 8 parts, zirconium white 9 parts and silicon nitride 5 parts.
Prepare rare earth doping phosphoric acid DFP biological 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 1380 DEG C, pressure 650MPa, time 6h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid DFP biological ceramics.
The block rare earth doping phosphoric acid DFP biological ceramics obtained is tested, detects the performance of biological ceramics: hardness 930HV; Compressive strength 1650MPa; Bending strength 660MPa; Toughness 16MPam 1/2.
Embodiment 4:
A kind of rare earth doping phosphoric acid DFP biological ceramics, comprises each component of following mass fraction:
Tricalcium phosphate 48 parts, Praseodymium trioxide 14 parts, ytterbium trichloride 6 parts, TiB2 5 parts, zirconium white 6 parts and silicon nitride 4 parts.
Prepare rare earth doping phosphoric acid DFP biological 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 1380 DEG C, pressure 650MPa, time 6h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid DFP biological ceramics.
The block rare earth doping phosphoric acid DFP biological ceramics obtained is tested, detects the performance of biological ceramics: hardness 940HV; Compressive strength 1650MPa; Bending strength 670MPa; Toughness 16MPam 1/2.
Embodiment 5:
A kind of rare earth doping phosphoric acid DFP biological ceramics, comprises each component of following mass fraction:
Tricalcium phosphate 54 parts, Praseodymium trioxide 17 parts, ytterbium trichloride 7 parts, TiB2 6 parts, zirconium white 8 parts and silicon nitride 4 parts.
Prepare rare earth doping phosphoric acid DFP biological 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 1380 DEG C, pressure 650MPa, time 5h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid DFP biological ceramics.
The block rare earth doping phosphoric acid DFP biological ceramics obtained is tested, detects the performance of biological ceramics: hardness 930HV; Compressive strength 1650MPa; Bending strength 670MPa; Toughness 16MPam 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 DFP biological ceramics, is characterized in that, is prepared from by each component of following mass fraction:
Tricalcium phosphate 42-62 part, Praseodymium trioxide 12-22 part, ytterbium trichloride 5-10 part, TiB2 3-8 part, zirconium white 5-10 part and silicon nitride 3-6 part.
2. rare earth doping phosphoric acid DFP biological ceramics according to claim 1, is characterized in that: the mass fraction of each component is: tricalcium phosphate 48-56 part, Praseodymium trioxide 14-18 part, ytterbium trichloride 6-8 part, TiB2 5-8 part, zirconium white 6-9 part and silicon nitride 4-5 part.
3. rare earth doping phosphoric acid DFP biological ceramics according to claim 2, is characterized in that: the mass fraction of each component is: tricalcium phosphate 54 parts, Praseodymium trioxide 17 parts, ytterbium trichloride 7 parts, TiB2 6 parts, zirconium white 8 parts and silicon nitride 4 parts.
4. a preparation method for rare earth doping phosphoric acid DFP biological 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 1100 DEG C-1500 DEG C, pressure 400-800MPa, time 3-10h;
(5), after calcining, taking-up to be cooled, namely obtains block rare earth doping phosphoric acid DFP biological ceramics.
5. the preparation method of rare earth doping phosphoric acid DFP biological ceramics according to claim 4, is characterized in that: in step (4), the temperature of calcining is 1380 DEG C.
6. the preparation method of rare earth doping phosphoric acid DFP biological ceramics according to claim 4, is characterized in that: in step (4), the pressure of calcining is 650MPa.
CN201510146659.2A 2015-03-31 2015-03-31 Rare-earth-doped tricalcium phosphate bioceramic and preparation method thereof Pending CN104744024A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105967662A (en) * 2016-05-06 2016-09-28 王泽陆 Alumina/strontia biological ceramic and preparation method thereof
CN109504555A (en) * 2018-11-28 2019-03-22 安徽尚尚家纺有限公司 A kind of natural feather sterilizing detergent for cleaning

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN102512706A (en) * 2011-12-16 2012-06-27 天津大学 Calcium polyphosphate/calcium sulfate complex phase biologic ceramic material and preparation method thereof

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN102512706A (en) * 2011-12-16 2012-06-27 天津大学 Calcium polyphosphate/calcium sulfate complex phase biologic ceramic material and preparation method thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105967662A (en) * 2016-05-06 2016-09-28 王泽陆 Alumina/strontia biological ceramic and preparation method thereof
CN109504555A (en) * 2018-11-28 2019-03-22 安徽尚尚家纺有限公司 A kind of natural feather sterilizing detergent for cleaning

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Application publication date: 20150701