CN1654428A - Method for preparing processable hydroxyapatite/Ti3SiC2 bioceramic composites - Google Patents
Method for preparing processable hydroxyapatite/Ti3SiC2 bioceramic composites Download PDFInfo
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- CN1654428A CN1654428A CN 200510008548 CN200510008548A CN1654428A CN 1654428 A CN1654428 A CN 1654428A CN 200510008548 CN200510008548 CN 200510008548 CN 200510008548 A CN200510008548 A CN 200510008548A CN 1654428 A CN1654428 A CN 1654428A
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Abstract
The present invention belongs to the field of biomedicine material technology, and is preparation process of composite hydroxyapatite/Ti3SiC2 bioceramic material. Ti3SiC2 and hydroxyapatite in certain ratio are mixed and sintered in non-oxidizing atmosphere or in vacuum state and at high temperature over 1250 deg.c to obtain the composite hydroxyapatite/Ti3SiC2 bioceramic material. The composite hydroxyapatite/Ti3SiC2 bioceramic material has high mechanical performance, including bending or breaking strength 70-300 MPa, toughness of 0.9-8 MPa.m1/2, elastic modulus 100-250 GPa and Vicker hardness 3-6 GPa; excellent machining property and excellent biomedical compatibility.
Description
Technical field
The invention belongs to the bio-medical material technical field, particularly a kind of processable hydroxyapatite/Ti silicon-carbon (Ti
3SiC
2) preparation method of biological ceramic composite material.
Background technology
A kind of bio-medical material that is applied to the mankind and other animal fields of hydroxyapatite has good biocompatibility, can be used for the bone reparation, fills, and the human body bone such as substitutes at purposes, and is with high content of technology, social demand is big.
Up to now, powder preparing and the sintering process to the hydroxylapatite biology medical material carried out a large amount of research-and-development activitys both at home and abroad, and obtained clinical application widely.But the strength ratio of present hydroxyapatite material is lower, can only be as the material of bone packing material and non-weight bearing area.Simultaneously, utilize the block body ceramic material of hydroxy apatite powder preparation to enbrittle, be difficult to shortcomings such as processing.
Processable hydroxyapatite/Ti silicon-carbon (Ti of the present invention
3SiC
2) biological ceramic composite material has mechanics and mechanical property and biocompatibility preferably, also has good processability simultaneously.Can be used to prepare people's skull bone, vertebrae, joint prosthesis etc.Prepare the block blank material by sintering, this material can accurately be processed at the geomery of clinical needs alternate sites according to patient, therefore has good clinical medical prospect.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of processable hydroxyapatite/Ti 3 SiC 2 bioceramic matrix material.It is characterized in that the preparation method of this biological ceramic composite material comprises following each step:
1) raw material is selected hydroxy apatite powder for use, and purity is not less than 99wt% (mass percent), and particle diameter is not more than 10 μ m; Titanium silicon-carbon purity is not less than 95wt% (mass percent), and particle diameter is not more than 10 μ m;
2) above-mentioned hydroxy apatite powder is mixed according to mass percent 10wt%～90wt% according to mass percent 90wt%～10wt% and titanium silicon-carbon powder, adopt mode thorough mixing such as ball milling or mechanical stirring;
3) adopt pressure or vibration pressure moulding to make blank above-mentioned compound;
4) above-mentioned blank is put into hot-pressed sintering furnace or non-pressure sintering furnace or microwave agglomerating furnace or discharge plasma sintering stove, feed sintering under rare gas element (purity is that mass percent is greater than 99.9wt%) or the vacuum state, at first with blank under above-mentioned atmosphere, heat-up rate is controlled at 10～50 ℃/minute, be warming up to 1250 ℃～1300 ℃ by room temperature, insulation naturally cools to room temperature more than 30 minutes then.
5) obtaining mechanical property is bending strength (or folding strength): 70～300MPa; Toughness: 0.9～8MPa.m
1/2Young's modulus: 100～250GPa; The hydroxyapatite/Ti 3 SiC 2 bioceramic composites of Vickers' hardness: 3～6GPa with good mechanical processing characteristics.
The invention has the beneficial effects as follows provides a kind of intensity, hardness, toughness and Young's modulus to adjust in a big way, can be used for the different mechanics of clinical needs and mechanical property, bio-medical novel material and the technology of preparing that can conveniently process.
Description of drawings
Fig. 1. under vacuum state, the relation of the bending strength of the processable hydroxyapatite/Ti 3 SiC 2 bioceramic matrix material of discharge plasma sintering, toughness and titanium silicon-carbon volumn concentration.
Fig. 2 under vacuum state, the relation of the Young's modulus of the processable hydroxyapatite/Ti 3 SiC 2 bioceramic matrix material of discharge plasma sintering, Vickers' hardness and titanium silicon-carbon volumn concentration.
Embodiment
The present invention proposes a kind of preparation method of processable hydroxyapatite/Ti 3 SiC 2 bioceramic matrix material.Specific embodiment is as follows: titanium silicon-carbon (Ti
3SiC
2) material is the harmless material of a kind of biology, have higher intensity and toughness, and have good processability; With itself and compoundization of hydroxyapatite with good biological medical science consistency, can significantly improve the strength and toughness (as shown in Figure 1, 2) of hydroxyapatite material, this matrix material has biomedical consistency and good processability simultaneously.The preparation method of this biological ceramic composite material comprises following each step:
1) raw material is selected hydroxy apatite powder for use, and purity is not less than 99wt% (mass percent), and particle diameter is not more than 10 μ m; Titanium silicon-carbon purity is not less than 95wt% (mass percent), and particle diameter is not more than 10 μ m;
2) above-mentioned hydroxy apatite powder is mixed according to mass percent 10wt%～90wt% according to mass percent 90wt%～10wt% and titanium silicon-carbon powder, adopt mode thorough mixing such as ball milling or mechanical stirring;
3) adopt pressure or vibration pressure moulding to make blank above-mentioned compound;
4) above-mentioned blank is put into hot-pressed sintering furnace or non-pressure sintering furnace or microwave agglomerating furnace or discharge plasma sintering stove, feed sintering under rare gas element (purity is that mass percent is greater than 99.9wt%) or the vacuum state, at first with blank under above-mentioned atmosphere, heat-up rate is controlled at 10～50 ℃/minute, be warming up to 1250 ℃ by room temperature, insulation naturally cools to room temperature more than 30 minutes then.
5) obtaining mechanical property is bending strength (or folding strength): 70～300MPa; Toughness: 0.9～8MPa.m
1/2Young's modulus: 100～250GPa; The hydroxyapatite/Ti 3 SiC 2 bioceramic composites of Vickers' hardness: 3～6GPa with good mechanical processing characteristics.For example the present invention is further specified below.
Embodiment one
Raw material is selected hydroxy apatite powder for use, and purity is not less than 99wt% (mass percent), and particle diameter is not more than 10 μ m; Titanium silicon-carbon (Ti
3SiC
2) purity is not less than 95wt% (mass percent), particle diameter is not more than 10 μ m.With hydroxy apatite powder according to volume percent 90% and titanium silicon-carbon (Ti
3SiC
2) powder mixes according to volume percent 10%, adopts the ball milling method thorough mixing; After making blank with pressure forming, put into hot-pressed sintering furnace, feed nitrogen (purity is that mass percent is greater than 99.9wt%), be warming up to 1250 ℃ by room temperature, be incubated 2 hours, naturally cool to room temperature then with 20 ℃/minute heat-up rates.Can obtain mechanical property is bending strength (or folding strength): 150MPa, toughness: 1.5MPa.m
1/2, Young's modulus: 105GPa, the processable hydroxyapatite/Ti silicon-carbon (Ti of Vickers' hardness: 5GPa
3SiC
2) biological ceramic composite material.
Embodiment two
Raw material is with embodiment one, with above-mentioned hydroxy apatite powder according to volume percent 70% and titanium silicon-carbon (Ti
3SiC
2) powder mixes according to volume percent 30%, adopts the ball milling method thorough mixing.Adopt pressure forming to make blank.Put into hot-pressed sintering furnace, after feeding argon gas (purity is that mass percent is greater than 99.9wt%) was pressed embodiment one sintering, obtaining mechanical property was bending strength (or folding strength): 200MPa, toughness: 3.2MPa.m
1/2, Young's modulus: 145GPa, the processable hydroxyapatite/Ti silicon-carbon (Ti of Vickers' hardness: 4.7GPa
3SiC
2) biological ceramic composite material.
Embodiment three
Raw material is with embodiment one, with above-mentioned hydroxy apatite powder according to volume percent 50% and titanium silicon-carbon (Ti
3SiC
2) powder mixes according to volume percent 50%, all the other obtain mechanical property after with embodiment one sintering is bending strength (or folding strength): 250MPa, toughness: 4.1MPa.m
1/2, Young's modulus: 160GPa, Vickers' hardness: 4.25GPa, the processable hydroxyapatite/Ti silicon-carbon (Ti of gpa
3SiC
2) biological ceramic composite material.
Embodiment four
Raw material is with embodiment one, with above-mentioned hydroxy apatite powder according to volume percent 90% and titanium silicon-carbon (Ti
3SiC
2) powder mixes according to volume percent 10%, adopt pressure forming to make blank, put into the spark plasma sintering stove, in vacuum tightness is under 100 pascals' the vacuum state, be warming up to 1250 ℃ of sintering with 20 ℃/minute heat-up rates, kept temperature 30 minutes, naturally cool to room temperature then, obtaining mechanical property is bending strength (or folding strength): 160MPa, toughness: 1.7MPa.m
1/2, Young's modulus: 115GPa, the processable hydroxyapatite/Ti silicon-carbon (Ti of Vickers' hardness: 5GPa
3SiC
2) biological ceramic composite material.
Embodiment five
Raw material is with embodiment one, with above-mentioned hydroxy apatite powder according to volume percent 70% and titanium silicon-carbon (Ti
3SiC
2) powder mixes according to volume percent 30%, adopt pressure forming to make blank, put into the spark plasma sintering stove, in vacuum tightness is under 100 pascals' the vacuum state, be warming up to 1250 ℃ of sintering with 20 ℃/minute heat-up rates, kept temperature 30 minutes, naturally cool to room temperature then, obtaining mechanical property is bending strength (or folding strength): 209MPa, toughness: 3.4MPa.m
1/2, Young's modulus: 150GPa, the processable hydroxyapatite/Ti silicon-carbon (Ti of Vickers' hardness: 4.6GPa
3SiC
2) biological ceramic composite material.
Embodiment six
Raw material is with embodiment one, with above-mentioned hydroxy apatite powder according to volume percent 50% and titanium silicon-carbon (Ti
3SiC
2) powder mixes according to volume percent 50%, adopt pressure forming to make blank, put into the spark plasma sintering stove, in vacuum tightness is under 100 pascals' the vacuum state, be warming up to 1250 ℃ of sintering with 20 ℃/minute heat-up rates, kept temperature 30 minutes, naturally cool to room temperature then, obtaining mechanical property is bending strength (or folding strength): 270MPa, toughness: 4.4MPa.m
1/2, Young's modulus: 180GPa, the processable hydroxyapatite/Ti silicon-carbon (Ti of Vickers' hardness: 4.35GPa
3SiC
2) biological ceramic composite material.
Embodiment seven
Raw material is with embodiment one, with hydroxy apatite powder according to volume percent 90% and titanium silicon-carbon (Ti
3SiC
2) powder is according to volume percent 10% mixing, employing ball milling method thorough mixing adopts pressure forming to make blank.Put into hot-pressed sintering furnace, feed argon gas (purity is that mass percent is greater than 99.9wt%), be 20 ℃/minute with heat-up rate and be warming up to 1300 ℃, kept temperature 2 hours, naturally cool to room temperature then by room temperature.Obtaining mechanical property is bending strength (or folding strength): 155MPa, toughness: 1.7MPa.m
1/2, Young's modulus: 112GPa, the processable hydroxyapatite/Ti silicon-carbon (Ti of Vickers' hardness: 4.9GPa
3SiC
2) biological ceramic composite material.
Embodiment eight
Raw material is with embodiment one, with hydroxy apatite powder according to volume percent 70% and titanium silicon-carbon (Ti
3SiC
2) powder is according to volume percent 30% mixing, employing ball milling method thorough mixing adopts pressure forming to make blank.Put into hot-pressed sintering furnace, feed argon gas (purity is that mass percent is greater than 99.9wt%), be 20 ℃/minute with heat-up rate and be warming up to 1300 ℃, kept temperature 2 hours, naturally cool to room temperature then by room temperature.Obtaining mechanical property is bending strength (or folding strength): 214MPa, toughness: 3.4MPa.m
1/2, Young's modulus: 150GPa, the processable hydroxyapatite/Ti silicon-carbon (Ti of Vickers' hardness: 4.8GPa
3SiC
2) biological ceramic composite material.
Embodiment nine
Raw material is with embodiment one, with hydroxy apatite powder according to volume percent 50% and titanium silicon-carbon (Ti
3SiC
2) powder is according to volume percent 50% mixing, employing ball milling method thorough mixing adopts pressure forming to make blank.Put into hot-pressed sintering furnace, feed argon gas (purity is that mass percent is greater than 99.9wt%), be 20 ℃/minute with heat-up rate and be warming up to 1300 ℃, kept temperature 2 hours, naturally cool to room temperature then by room temperature.Obtaining mechanical property is bending strength (or folding strength): 260MPa, toughness: 4.3MPa.m
1/2, Young's modulus: 170GPa, the processable hydroxyapatite/Ti silicon-carbon (Ti of Vickers' hardness: 4.25GPa
3SiC
2) biological ceramic composite material.
Claims (2)
1. the preparation method of a processable hydroxyapatite/Ti 3 SiC 2 bioceramic matrix material is characterized in that, the preparation method of this biological ceramic composite material comprises following each step:
1) raw material is selected hydroxy apatite powder for use, and purity is not less than 99wt% (mass percent), and particle diameter is not more than 10 μ m; Titanium silicon-carbon purity is not less than 95wt% (mass percent), and particle diameter is not more than 10 μ m;
2) above-mentioned hydroxy apatite powder is mixed according to mass percent 10wt%～90wt% according to mass percent 90wt%～10wt% and titanium silicon-carbon powder, adopt mode thorough mixing such as ball milling or mechanical stirring;
3) adopt pressure or vibration pressure moulding to make blank above-mentioned compound;
4) above-mentioned blank put into hot-pressed sintering furnace or non-pressure sintering furnace or microwave agglomerating furnace or discharge plasma sintering stove, feed sintering under rare gas element (purity is that mass percent is greater than 99.9wt%) or the vacuum state, at first with blank under above-mentioned atmosphere, heat-up rate is controlled at 10～50 ℃/minute, be warming up to 1250 ℃～1300 ℃ by room temperature, insulation is more than 30 minutes, naturally cool to room temperature then, obtaining mechanical property is bending strength (or folding strength): 70～300MPa; Toughness: 0.9～8 MPa.m
1/2Young's modulus: 100～250GPa; The hydroxyapatite/Ti 3 SiC 2 bioceramic composites of Vickers' hardness: 3～6GPa with good mechanical processing characteristics.
2. according to the preparation method of the described processable hydroxyapatite/Ti 3 SiC 2 bioceramic matrix material of claim 1, it is characterized in that: described use rare gas element argon gas or nitrogen.
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|---|---|---|---|
| CN 200510008548 CN1282629C (en) | 2005-02-22 | 2005-02-22 | Method for preparing processable hydroxyapatite/Ti3SiC2 bioceramic composites |
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|---|---|---|---|
| CN 200510008548 CN1282629C (en) | 2005-02-22 | 2005-02-22 | Method for preparing processable hydroxyapatite/Ti3SiC2 bioceramic composites |
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| CN1282629C CN1282629C (en) | 2006-11-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100554216C (en) * | 2007-12-11 | 2009-10-28 | 北京科技大学 | A kind of method that adopts the microwave method synthesizing barium ferrocobalt niobium oxide material |
| CN101791428A (en) * | 2010-03-17 | 2010-08-04 | 天津大学 | Magnesium/hydroxyapatite composite material and preparation method thereof |
| CN102303977A (en) * | 2011-05-24 | 2012-01-04 | 东北大学 | Method for preparing titanium-iron particle reinforced hydroxyapatite-based bioceramic material |
| CN107708650A (en) * | 2015-07-13 | 2018-02-16 | 三仪股份有限公司 | Dental surface film formation powder comprising the apatite through burning till |
-
2005
- 2005-02-22 CN CN 200510008548 patent/CN1282629C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100554216C (en) * | 2007-12-11 | 2009-10-28 | 北京科技大学 | A kind of method that adopts the microwave method synthesizing barium ferrocobalt niobium oxide material |
| CN101791428A (en) * | 2010-03-17 | 2010-08-04 | 天津大学 | Magnesium/hydroxyapatite composite material and preparation method thereof |
| CN101791428B (en) * | 2010-03-17 | 2013-03-13 | 天津大学 | Magnesium/hydroxyapatite composite material and preparation method thereof |
| CN102303977A (en) * | 2011-05-24 | 2012-01-04 | 东北大学 | Method for preparing titanium-iron particle reinforced hydroxyapatite-based bioceramic material |
| CN107708650A (en) * | 2015-07-13 | 2018-02-16 | 三仪股份有限公司 | Dental surface film formation powder comprising the apatite through burning till |
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| Publication number | Publication date |
|---|---|
| CN1282629C (en) | 2006-11-01 |
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