CN104496459B - A kind of Nano-grained Hydroxyapatite Ceramics and preparation method thereof - Google Patents
A kind of Nano-grained Hydroxyapatite Ceramics and preparation method thereof Download PDFInfo
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- CN104496459B CN104496459B CN201410713067.XA CN201410713067A CN104496459B CN 104496459 B CN104496459 B CN 104496459B CN 201410713067 A CN201410713067 A CN 201410713067A CN 104496459 B CN104496459 B CN 104496459B
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Abstract
The present invention relates to a kind of Nano-grained Hydroxyapatite Ceramics and preparation method thereof, belong to ceramic processing technique field, the weight portion of the most each component is hydroxyapatite 20～50 parts, Al2O340～60 parts, CaO 10～20 parts, ZrO21～10 part, Y2O31～10 part, CaF21～10 part, its preparation method is by after said components in proportion dispensing, add alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 70 ~ 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 ~ 1200 DEG C of process 8 ~ 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove；This Nano-grained Hydroxyapatite Ceramics is three-dimensional porous foams shape, porosity of=90%, is suitable for timbering material and the bone renovating material of bone tissue engineer.
Description
Technical field
The present invention relates to a kind of pottery and preparation method thereof, be specifically related to a kind of Nano-grained Hydroxyapatite Ceramics material and preparation method thereof, belong to ceramic processing technique field.
Background technology
Since nearly half a century people hanker after bioceramic sclerous tissues research main reason is that: the operation wound of (1) autologous bone transplanting and possible complication；(2) the potential disease infection risk of allogenic bone transplantation；(3) find that osseous tissue can organically combine with the bioceramic of some calcics；(4) development of bioceramic technology of preparing.Hydroxyapatite is the main inorganic composition of skeleton, it it is the class bioactive materials with good biocompatibility, after implanting osseous tissue, chemical that can be the strongest with bone formation on interface is bonded, there is bone conduction and osteoinductive, be therefore one of important thing implanting bioceramic material research.The heat stability of nanometer hydroxyapatite directly affects mechanical property and the Biofunctional of ceramic material, therefore, one of factor study hotspot becoming this field affecting nanometer hydroxyapatite heat stability.
The performance of ceramic material is closely related with crystallite dimension, and the size of crystal grain is relevant to the particle diameter of material powder, so the preparation of powder body is particularly important.The preparation method of hydroxyapatite mainly has at present: the methods such as Hydrothermal Synthesis, sol-gel, solid state reaction, co-precipitation, mechanochemistry ball milling.Since 1986
Gedye and Giguere etc. have reported household microwave oven since synthesis of organic substance, microwave because of can improve chemical reaction response speed, can suppress under certain conditions the carrying out of reaction and change the approach of reaction, easy and simple to handle, by-product is few, productivity is high and saves the advantages such as the energy makes microwave-assisted synthesis be developed rapidly.Microwave is widely used to from inorganic reaction to organic reaction now, from medication chemistry to food chemistry, from simple molecules to fields such as complicated life processes.But the report preparing high temperatures nano-hydroxy-apatite both at home and abroad is the most few.
The mechanical performance of tradition hydroxylapatite ceramic is poor, and such as, fracture toughness (KIC) does not surpass 1.0MPa.m1/2, poor as its dependability of artificial growth body.Up to the present, HAP pottery cannot act as supportive implant, and its application medically is only limitted to powder, coating and the stephanoporate implant of low carrying.Nano-biological cerimic is little due to crystal grain, makes the inherent pore in material or flaw size greatly reduce, and does not easily cause transgranular fracture, and is conducive to improving the fracture toughness of material；Meanwhile, the refinement of crystal grain makes again number of grain boundaries be greatly increased, and contributes to intercrystalline sliding, makes nano-biological cerimic show the mechanical properties such as unique superplasticity.
201310148908.2 disclose a kind of porous nano pottery built by hydroxyapatite nano rod or sheet and preparation method, the method is, by hydro-thermal method, phosphoric acid DFP porous ceramics is carried out nanorize, it is thus achieved that the porous nano pottery built by hydroxyapatite nano rod or nanometer sheet；But the method is higher to the requirement of equipment, so that this patent exists one-time investment height, product cost is difficult to the problems such as reduction；The present invention is with hydroxyapatite, Al2O3、CaO、ZrO2、Y2O3、CaF2Deng for raw material, prepared Nano-grained Hydroxyapatite Ceramics has higher biological activity, and improves its degradability, and preparation method is simple, and repeatability is high, can be with large-scale production.
Summary of the invention
It is an object of the invention to provide a kind of Nano-grained Hydroxyapatite Ceramics, this Nano-grained Hydroxyapatite Ceramics has higher biological activity, and improves its degradability, and preparation method is simple, and repeatability is high, can be with large-scale production.
In order to solve the problems referred to above, the technical solution adopted in the present invention is:
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 20～50 parts, Al2O340～60 parts, CaO 10～20 parts, ZrO2
1～10 part, Y2O3
1～10 part, CaF2
1～10 part.
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 25～30 parts, Al2O340～45 parts, CaO 15～20 parts, ZrO2
2～3 parts, Y2O3
2～4 parts, CaF2
4～5 parts.
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 30～35 parts, Al2O345～50 parts, CaO 10～15 parts, ZrO2
5～6 parts, Y2O36～8 parts, CaF2
2～3 parts.
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 35～40 parts, Al2O350～55 parts, CaO 15～18 parts, ZrO2
6～8 parts, Y2O3
8～9 parts, CaF2
2～3 parts.
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 40～45 parts, Al2O355～60 parts, CaO 18～20 parts, ZrO2
8～10 parts, Y2O3
8～10 parts, CaF2
4～6 parts.
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 45～50 parts, Al2O340～55 parts, CaO 10～14 parts, ZrO2
2～5 parts, Y2O36～7 parts, CaF2
5～8 parts.
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 30～40 parts, Al2O340～50 parts, CaO 10～15 parts, ZrO2
6～7 parts, Y2O3
7～8 parts, CaF2
3～5 parts.
The preparation method of a kind of Nano-grained Hydroxyapatite Ceramics, comprises the steps:
After said components in proportion dispensing, add appropriate alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 70 ~ 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 ~ 1200 DEG C of process 8 ~ 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
The present invention provides the benefit that relative to prior art:
The Nano-grained Hydroxyapatite Ceramics that the present invention prepares has higher biological activity, and improves its degradability, and preparation method is simple, and repeatability is high, can be with large-scale production.
Detailed description of the invention
Being described in further details the present invention below by embodiment, these embodiments are only used for the present invention is described, do not limit the scope of the invention.
Embodiment
1
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 20 parts, Al2O360 parts, CaO 10 parts, ZrO2
5 parts, Y2O35 parts, CaF25 parts.
Its preparation method, comprises the following steps:
After said components in proportion dispensing, add alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 80 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 DEG C of process 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
Embodiment
2
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 25 parts, Al2O340 parts, CaO20 part, ZrO2
10 parts, Y2O38 parts, CaF21～10 part.
Its preparation method, comprises the following steps:
After said components in proportion dispensing, add alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 85 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 DEG C of process 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
Embodiment
3
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 30 parts, Al2O350 parts, CaO 15 parts, ZrO26 parts, Y2O36 parts, CaF25 parts.
Its preparation method, comprises the following steps:
After said components in proportion dispensing, add alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 85 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1200 DEG C of process 8h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
Embodiment
4
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 40 parts, Al2O345 parts, CaO 18 parts, ZrO2
6 parts, Y2O37 parts, CaF24 parts.
Its preparation method, comprises the following steps:
After said components in proportion dispensing, add alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 85 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1100 DEG C of process 9h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
Embodiment
5
A kind of Nano-grained Hydroxyapatite Ceramics, is made up of the component of following weight portion:
Hydroxyapatite 50 parts, Al2O340 parts, CaO 10 parts, ZrO28 parts, Y2O38 parts, CaF25 parts.
Its preparation method, comprises the following steps:
After said components in proportion dispensing, add alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1200 DEG C of process 8h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
Claims (7)
1. a Nano-grained Hydroxyapatite Ceramics, it is characterised in that: it is made up of the component of following weight portion:
Hydroxyapatite 20～50 parts, Al2O340～60 parts, CaO
10～20 parts, ZrO2
1～10 part, Y2O3
1～10 part, CaF2
1～10 part；
Its step is as follows:
After said components in proportion dispensing, add appropriate alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 70 ~ 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 ~ 1200 DEG C of process 8 ~ 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
2. a Nano-grained Hydroxyapatite Ceramics, it is characterised in that: it is made up of the component of following weight portion:
Hydroxyapatite 25～30 parts, Al2O340～45 parts, CaO
15～20 parts, ZrO2
2～3 parts, Y2O3
2～4 parts, CaF2
4～5 parts；
Its step is as follows:
After said components in proportion dispensing, add appropriate alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 70 ~ 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 ~ 1200 DEG C of process 8 ~ 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
3. a Nano-grained Hydroxyapatite Ceramics, it is characterised in that: it is made up of the component of following weight portion:
Hydroxyapatite 30～35 parts, Al2O345～50 parts, CaO
10～15 parts, ZrO2
5～6 parts, Y2O36～8 parts, CaF2
2～3 parts；
Its step is as follows:
After said components in proportion dispensing, add appropriate alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 70 ~ 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 ~ 1200 DEG C of process 8 ~ 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
4. a Nano-grained Hydroxyapatite Ceramics, it is characterised in that: it is made up of the component of following weight portion:
Hydroxyapatite 35～40 parts, Al2O350～55 parts, CaO
15～18 parts, ZrO2
6～8 parts, Y2O3
8～9 parts, CaF2
2～3 parts；
Its step is as follows:
After said components in proportion dispensing, add appropriate alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 70 ~ 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 ~ 1200 DEG C of process 8 ~ 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
5. a Nano-grained Hydroxyapatite Ceramics, it is characterised in that: it is made up of the component of following weight portion:
Hydroxyapatite 40～45 parts, Al2O355～60 parts, CaO
18～20 parts, ZrO2
8～10 parts, Y2O3
8～10 parts, CaF2
4～6 parts；
Its step is as follows:
After said components in proportion dispensing, add appropriate alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 70 ~ 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 ~ 1200 DEG C of process 8 ~ 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
6. a Nano-grained Hydroxyapatite Ceramics, it is characterised in that: it is made up of the component of following weight portion:
Hydroxyapatite 45～50 parts, Al2O340～55 parts, CaO
10～14 parts, ZrO2
2～5 parts, Y2O36～7 parts, CaF2
5～8 parts；
Its step is as follows:
After said components in proportion dispensing, add appropriate alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 70 ~ 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 ~ 1200 DEG C of process 8 ~ 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
7. a Nano-grained Hydroxyapatite Ceramics, it is characterised in that: it is made up of the component of following weight portion:
Hydroxyapatite 30～40 parts, Al2O340～50 parts, CaO
10～15 parts, ZrO2
6～7 parts, Y2O3
7～8 parts, CaF2
3～5 parts；
Its step is as follows:
After said components in proportion dispensing, add appropriate alcoholic solution uniformly to mix, mediate, then in 80 DEG C of water-baths, evaporate solvent, the baking oven of 70 ~ 90 DEG C is heated foaming, base substrate after moldings formed therefrom is placed in Muffle furnace and is to slowly warm up to 1000 ~ 1200 DEG C of process 8 ~ 10h, and cooling obtains Nano-grained Hydroxyapatite Ceramics finished product after coming out of the stove.
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| CN105036747A (en) * | 2015-06-25 | 2015-11-11 | 合肥蓝科新材料有限公司 | Nano-hydroxyapatite-doped high-density motor carbon brush material and preparation method thereof |
| CN106045495B (en) * | 2016-05-25 | 2018-07-03 | 西南科技大学 | A kind of porous fluor-apatite ceramic preparation of Adsorption of Radioactive nucleic |
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| JPH0670658A (en) * | 1992-08-25 | 1994-03-15 | Sangi Co Ltd | Pearl nucleus to be used in pearl culture |
| CN1397518A (en) * | 2002-08-28 | 2003-02-19 | 中国科学院长春应用化学研究所 | Process for preparing nano-class hydroxyphosphorite/alumina bioceramics |
| CN1927769A (en) * | 2005-09-06 | 2007-03-14 | 四川大学 | Preparation method and apparatus of nano porous biologic ceramics |
| CN102000361A (en) * | 2010-11-02 | 2011-04-06 | 陕西科技大学 | Preparation method of HA (Hydroxyapatite)-beta-tricalcium phosphate-alumina three-phase composite bioceramic |
| WO2013004361A2 (en) * | 2011-07-06 | 2013-01-10 | Nobel Biocare Services Ag | Composite ceramic for dental implants |
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2014
- 2014-12-02 CN CN201410713067.XA patent/CN104496459B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0670658A (en) * | 1992-08-25 | 1994-03-15 | Sangi Co Ltd | Pearl nucleus to be used in pearl culture |
| CN1397518A (en) * | 2002-08-28 | 2003-02-19 | 中国科学院长春应用化学研究所 | Process for preparing nano-class hydroxyphosphorite/alumina bioceramics |
| CN1927769A (en) * | 2005-09-06 | 2007-03-14 | 四川大学 | Preparation method and apparatus of nano porous biologic ceramics |
| CN102000361A (en) * | 2010-11-02 | 2011-04-06 | 陕西科技大学 | Preparation method of HA (Hydroxyapatite)-beta-tricalcium phosphate-alumina three-phase composite bioceramic |
| WO2013004361A2 (en) * | 2011-07-06 | 2013-01-10 | Nobel Biocare Services Ag | Composite ceramic for dental implants |
Non-Patent Citations (1)
| Title |
|---|
| 羟基磷灰石/TiO2纳米管复合生物相容性;张杭州等;《中国组织工程研究》;20140331(第3期);全文 * |
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