CN106542845A - Hydroxyapatite overlong nanowire porous ceramicss and preparation method thereof - Google Patents
Hydroxyapatite overlong nanowire porous ceramicss and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to hydroxyapatite overlong nanowire porous ceramicss and preparation method thereof, the hydroxyapatite overlong nanowire porous ceramicss are prepared from as raw material by hydroxyapatite overlong nanowire.The present invention prepares a kind of hydroxyapatite overlong nanowire porous ceramicss with excellent biocompatibility, three-dimensional communication pore passage structure and high porosity as raw material by the use of hydroxyapatite overlong nanowire first.
Description
Technical field
The present invention relates to a kind of hydroxyapatite overlong nanowire porous ceramicss with three-dimensional communication pore passage structure, specifically
It is related to using hydroxyapatite overlong nanowire as raw material, using palmitic acid as pore creating material, by molding, sintering is prepared has
The hydroxyapatite overlong nanowire porous ceramicss of three-dimensional communication pore passage structure, pore size and porosity can be added by pore creating material
Dosage is regulating and controlling.The invention belongs to ceramic material preparation field.
Background technology
Porous ceramicss with excellent biocompatibility, three-dimensional communication pore passage structure have important in biomedical sector
Using value, can be used as bone impairment renovation material.Therefore, with excellent biocompatibility, three-dimensional communication pore passage structure it is many
Hole ceramics are received more and more attention.
Up to the present, people have synthesized the hydroxyl with different porosities by various different synthetic methods
Apatite porous ceramicss, including sol-gel, gel injection-moulding, freeze-dried and the addition method such as pore creating material.But for hydroxyl
Research of the pattern of base apatite to prepared porous ceramicss performance impact is also rarely reported.
Although the synthetic method of the existing hydroxyapatite porous ceramicss of document is reported at present, in order to obtain high porosity
Hydroxyapatite porous ceramicss, its preparation method is more complicated, and mostly with hydroxyapatite nanoparticle as raw material, institute
The porosity or/and pore passage structure for obtaining hydroxyapatite porous ceramicss is undesirable.By the use of hydroxyapatite overlong nanowire as
Raw material prepares hydroxyapatite porous ceramicss and has not been reported.
The content of the invention
For the problems referred to above, it is an object of the invention to provide a kind of have excellent biocompatibility, three-dimensional communication duct
The hydroxyapatite overlong nanowire porous ceramicss of structure and high porosity.
On the one hand, the invention provides a kind of hydroxyapatite overlong nanowire porous ceramicss, the hydroxyapatite surpasses
Long nano wire porous ceramicss are prepared from as raw material by hydroxyapatite overlong nanowire.
The present invention first using hydroxyapatite overlong nanowire as raw material prepare it is a kind of with excellent biocompatibility,
The hydroxyapatite overlong nanowire porous ceramicss of three-dimensional communication pore passage structure and high porosity.Compare hydroxyapatite nano
Grain, hydroxyapatite overlong nanowire has high length-diameter ratio, in the preparation process of porous ceramicss, even if adding substantial amounts of making
Hole agent, due to the interaction between nano wire and nano wire, ceramic body will not also cave in sintering process.
It is preferred that the hydroxyapatite overlong nanowire porous ceramicss have three-dimensional communication pore passage structure, channel diameter
And adjustable porosity.
It is preferred that the length of the hydroxyapatite overlong nanowire is 30~1000 microns, a diameter of 5~100 nanometers.
On the other hand, the present invention provides the preparation method of above-mentioned hydroxyapatite overlong nanowire porous ceramicss, including:Will
Hydroxyapatite overlong nanowire and pore creating material uniformly mix, and Jing after molding, sintering obtain the hydroxyapatite overlength nanometer
Line porous ceramicss.
It is preferred that the pore creating material be the organic pore-forming agents that can decompose at a certain temperature or with inorganic pore creating material, it is excellent
Elect palmitic acid as.
It is preferred that the mass ratio of the hydroxyapatite overlong nanowire and pore creating material is 10:1~1:10.
The present invention can also pass through the content and size for controlling pore creating material, and hydroxyapatite overlong nanowire porous can be made pottery
Porcelain pore size and porosity can be regulated and controled by pore creating material.
It is preferred that described, to be shaped to tablet machine dry-pressing formed.
Also, it is preferred that the pressure of the molding is 1~50MPa.
It is preferred that the atmosphere of the sintering is air atmosphere.
It is preferred that the temperature of the sintering is 800~1600 DEG C, sintering time is more than 5 minutes.Also, it is preferred that the burning
Heating rate during knot is 1~50 DEG C/min, preferably 2~10 DEG C/min.
The hydroxyapatite with excellent biocompatibility, three-dimensional communication pore passage structure and high porosity that the present invention is provided
Overlong nanowire porous ceramicss, its pore size and porosity can be regulated and controled by pore creating material.
The obtained hydroxyapatite with excellent biocompatibility, three-dimensional communication pore passage structure and high porosity of the invention
Overlong nanowire porous ceramicss can be applicable to the multiple fields such as such as biomedical sector.System of the present invention to extension porous ceramicss
Standby and application is with important scientific meaning and practical value.
Also, the preparation process is simple of the present invention, easy to operate, it is not necessary to the equipment of complex and expensive, it is expected to realize industrialization.
Hydroxyapatite overlong nanowire with excellent biocompatibility, three-dimensional communication pore passage structure and high porosity of the present invention
Porous ceramicss have a good application prospect in multiple fields such as biomedicines.
Description of the drawings
Fig. 1 is that the scanning electron for adding hydroxyapatite overlong nanowire porous ceramicss prepared by different content pore creating material shows
Micro- (SEM) photo;
Fig. 2 spreads out for the X-ray of hydroxyapatite overlong nanowire and its porous ceramicss, hydroapatite particles and its sintered product
Penetrate (XRD) figure;
Fig. 3 is to add hydroxyapatite overlong nanowire porous ceramicss (upper to arrange) and hydroxy-apatite prepared by different content pore creating material
The digital photograph of the material (lower to arrange) prepared after stone granule sintering.
Specific embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, and the unrestricted present invention.
The present invention using hydroxyapatite overlong nanowire as raw material, with palmitic acid or other it at a certain temperature can be with
Organic and inorganic pore creating material for decomposing etc. is prepared with excellent biocompatibility, three-dimensional by molding, sintering as pore creating material
The hydroxyapatite overlong nanowire porous ceramicss of connected pore channel structure and high porosity.
Hydroxyapatite overlong nanowire porous ceramicss prepared by the present invention have three-dimensional communication pore passage structure, channel diameter
Porosity can scalable.
In the present invention, the length range of the hydroxyapatite overlong nanowire is 30 microns~1000 microns, nano wire
A diameter of 5 nanometers~100 nanometers.
The preparation method of the hydroxyapatite overlong nanowire porous ceramicss that the explanation present invention in following exemplary ground is provided.
Hydroxyapatite overlong nanowire of the present invention can be prepared using solvent-thermal method, refer to document and patent report
It is prepared by the method in road:Zhu Yingjie, Lu Bingqiang, Chen Feng, hydroxyapatite paper that high-flexibility high temperature resistant is not fired and preparation method thereof,
The patent No.:ZL201310687363.2;Ying-Ying Jiang,Ying-Jie Zhu*,Feng Chen,Jin Wu,
Ceramics International,41,6098-6102(2015);Yong-Gang Zhang,Ying-Jie Zhu*Feng
Chen,Jin Wu,Materials Letters,144,135-137(2015).Other suitable preparation methoies, institute may also be employed
As long as do not limited with method to prepare the hydroxyapatite overlong nanowire.
Hydroxyapatite overlong nanowire and pore creating material are uniformly mixed, Jing after molding at 800~1600 DEG C (preferably 1000
~1300 DEG C) under sintering more than 5 minutes (preferably 1 hour~5 hours), obtain the hydroxyapatite overlong nanowire porous pottery
Porcelain.Specifically, weigh certain mass hydroxyapatite overlong nanowire and pore creating material (for example, palmitic acid, other are organic,
Inorganic pore creating material etc.) mix homogeneously.And using certain molding mode carry out molding (as tablet machine is dry-pressing formed, isostatic pressed into
Type etc.).Using being burnt under conditions of certain sintering processing (as Muffle furnace is normal pressure-sintered under air atmosphere) and experiment parameter
Knot.Preferably, heating rate can be 1 degrees celsius/minute~50 degrees celsius/minute.Temperature retention time is more than 5 minutes.Holding temperature
For 800 degrees Celsius~1600 degrees Celsius.Can obtain with excellent biocompatibility, three-dimensional communication hole after temperature is down to room temperature
The hydroxyapatite overlong nanowire porous ceramicss of road structure and high porosity.
For forming and sintering, specifically, hydroxyapatite overlong nanowire is uniformly mixed with pore creating material, tabletting is put into
In grinding tool (for example, stainless steel mould), molding under a certain pressure is then transferred them in sintering furnace, in certain intensification
It is sintered under the conditions of speed, temperature retention time, holding temperature.
Molding can be dry-pressing formed using tablet machine, and briquetting pressure can be 1~50MPa.Sintering can be using normal under air atmosphere
Pressure sintering (pressureless sintering under air atmosphere), it should be understood that other molding and sintering processing can also be used.Wherein, forming and sintering
When, briquetting pressure and sintering temperature scalable, such as briquetting pressure 8MPa, sintering temperature are 1300 degrees Celsius.
In the present invention, the mass ratio of the hydroxyapatite overlong nanowire and pore creating material can be according to required pore size
Selected with porosity, for example, can be 1:10~10:1.Usage amount and/or size of the present invention by control pore creating material, can
Regulated and controled with the pore size (channel diameter) and porosity to the hydroxyapatite overlong nanowire porous ceramicss, more
Hydroxyapatite overlong nanowire with excellent biocompatibility, three-dimensional communication pore passage structure and high porosity is obtained easily
Porous ceramicss.For example, when the usage amount of pore creating material is improved, porosity can be increased;When the size of pore creating material is increased, can be with
Increase pore size and porosity.Vice versa.In the present invention, it is possible to use substantial amounts of pore creating material is obtaining high porosity, example
Mass ratio such as hydroxyapatite overlong nanowire and pore creating material can be 1:10.When using substantial amounts of pore creating material, due to nanometer
Interaction between line and nano wire, ceramic body will not be caved in sintering process.
The invention has the advantages that:
(1) preparation method is simple, it is not necessary to the equipment of complex and expensive, is expected to realize industrialization;
(2) hydroxyapatite with excellent biocompatibility, three-dimensional communication pore passage structure and high porosity can be prepared to surpass
Long nano wire porous ceramicss;
(3) aperture of hydroxyapatite overlong nanowire porous ceramicss obtained by being adjusted as the content of pore creating material and size
Size and porosity and do not destroy its structure.
Hydroxyapatite overlong nanowire porous ceramicss of the present invention are by hydroxyapatite overlong nanowire as original
Material is prepared from, and which has excellent biocompatibility, three-dimensional communication pore passage structure and high porosity, in multiple necks such as biomedicine
Domain has a good application prospect.
The present invention surveys the aperture of hydroxyapatite overlong nanowire porous ceramicss, porosity by Archimedes's drainage.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only that an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Production Example 1
At room temperature, respectively by 0.1760g CaCl2、0.3480g NaH2PO4, 0.700g NaOH be dissolved in 10mL deionized waters
In.30min will be mixed under 9mL deionized waters, 4mL methanol, 7mL Oleic acid magnetic agitation, be added dropwise over 10mL afterwards successively
CaCl2Solution, 10mL NaOH solutions, 10mLNaH2PO4Solution, continues stirring 30min.Then this mixed solution is transferred to
In 100mL reactors, sealing, after 180 DEG C of reaction 24h, naturally cools to room temperature, and product is precipitated in ethanol, then with water, ethanol
With hexamethylene cyclic washing repeatedly, until hydroxyapatite overlong nanowire water slurry pH is close to 7.4, protect at 4 DEG C afterwards
Deposit.Finally give hydroxyapatite overlong nanowire.
Embodiment 1
At room temperature, by 100 milligrams of hydroxyapatite overlong nanowires and 350 milligrams of pore creating material palmitic acid, (particle diameter 300-700 is micro-
Rice) mix homogeneously, and put in a diameter of 10 millimeters of stainless steel mould, a diameter of 10 millimeters are depressed in 8MPa pressure
Disk, then the disk for pressing is put into it is normal pressure-sintered in air atmosphere in Muffle furnace, heating rate be 10 degrees celsius/minutes,
And sinter 4 hours under 1300 degrees Celsius, finally obtain with excellent biocompatibility, three-dimensional communication pore passage structure and high hole
The hydroxyapatite overlong nanowire porous ceramicss of rate, as shown in I in Fig. 3 (a).Hydroxyapatite overlong nanowire obtained by wherein
The porosity of porous ceramicss is 89%.
Embodiment 2
At room temperature, by 100 milligrams of hydroxyapatite overlong nanowires and 250 milligrams of pore creating material palmitic acid, (particle diameter 300-700 is micro-
Rice) mix homogeneously, and put in a diameter of 10 millimeters of stainless steel mould, a diameter of 10 millimeters are depressed in 8MPa pressure
Disk, then the disk for pressing is put into it is normal pressure-sintered in air atmosphere in Muffle furnace, heating rate be 10 degrees celsius/minutes,
And sinter 4 hours under 1300 degrees Celsius, finally obtain with excellent biocompatibility, three-dimensional communication pore passage structure and high hole
The hydroxyapatite overlong nanowire porous ceramicss of rate, as shown in II in Fig. 3 (a).Hydroxyapatite overlength nanometer obtained by wherein
The porosity of line porous ceramicss is 84%.
Embodiment 3
At room temperature, by 100 milligrams of hydroxyapatite overlong nanowires and 150 milligrams of pore creating material palmitic acid, (particle diameter 300-700 is micro-
Rice) mix homogeneously, and put in a diameter of 10 millimeters of stainless steel mould, a diameter of 10 millimeters are depressed in 8MPa pressure
Disk, then the disk for pressing is put into it is normal pressure-sintered in air atmosphere in Muffle furnace, heating rate be 10 degrees celsius/minutes,
And sinter 4 hours under 1300 degrees Celsius, finally obtain with excellent biocompatibility, three-dimensional communication pore passage structure and high hole
The hydroxyapatite overlong nanowire porous ceramicss of rate, as shown in III in Fig. 3 (a).Hydroxyapatite overlength nanometer obtained by wherein
The porosity of line porous ceramicss is 76%.
Comparative example 1
At room temperature, by 100 milligrams of hydroxyapatite nanoparticles and 350 milligrams of pore creating material palmitic acid, (particle diameter 300-700 is micro-
Rice) mix homogeneously, and put in a diameter of 10 millimeters of stainless steel mould, a diameter of 10 millimeters are depressed in 8MPa pressure
Disk, then the disk for pressing is put into it is normal pressure-sintered in air atmosphere in Muffle furnace, heating rate be 10 degrees celsius/minutes,
And sinter 4 hours under 1300 degrees Celsius.Blank structure collapses into powder body completely, it is impossible to obtain porous ceramicss, I in such as Fig. 3 (b)
It is shown.
Comparative example 2
Will be 100 milligrams of hydroxyapatite nanoparticles and 250 milligrams of pore creating material palmitic acid (particle diameter 300-700 microns) mixing equal
It is even, and put in a diameter of 10 millimeters of stainless steel mould, a diameter of 10 millimeters of disk is depressed in 8MPa pressure, then will
The disk for pressing is put into normal pressure-sintered in air atmosphere in Muffle furnace, and heating rate is 10 degrees celsius/minutes, and is taken the photograph 1300
Sinter 4 hours under family name's degree.Blank structure collapses into powder body completely, it is impossible to obtain porous ceramicss, as shown in II in Fig. 3 (b).
Comparative example 3
Will be 100 milligrams of hydroxyapatite nanoparticles and 150 milligrams of pore creating material palmitic acid (particle diameter 300-700 microns) mixing equal
It is even, and put in a diameter of 10 millimeters of stainless steel mould, a diameter of 10 millimeters of disk is depressed in 8MPa pressure, then will
The disk for pressing is put into normal pressure-sintered in air atmosphere in Muffle furnace, and heating rate is 10 degrees celsius/minutes, and is taken the photograph 1300
Sinter 4 hours under family name's degree.Blank structure collapses into powder body completely, it is impossible to obtain porous ceramicss, as shown in III in Fig. 3 (b).
Fig. 1 is that the scanning electron for adding hydroxyapatite overlong nanowire porous ceramicss prepared by different content pore creating material shows
Micro- (SEM) photo, wherein figure a1, a2, a3 are respectively pore creating material addition being obtained under ceramic different amplification by 150 milligrams
Electron scanning micrograph;B1, b2, b3 are respectively pore creating material addition and obtain ceramics difference times magnification by 250 milligrams
Electron scanning micrograph under several;C1, c2, c3 are respectively pore creating material addition and are put by 350 milligrams of acquisition ceramics differences
Electron scanning micrograph under big multiple.As can be known from Fig. 1 as Content of Pore-forming Agents increases, gained hydroxyapatite overlength
The pore distribution of nano wire porous ceramicss it is more uniform.1-3 understands to increase with Content of Pore-forming Agents in conjunction with the embodiments, gained hydroxyl
The porosity of base apatite overlong nanowire porous ceramicss gradually increases.
Fig. 2 is hydroxyapatite overlong nanowire, hydroxyapatite overlong nanowire porous ceramicss, hydroapatite particles
And its X-ray diffraction (XRD) figure of sintered product.It can be seen that hydroxyapatite overlong nanowire, hydroxyapatite overlength
Nano wire porous ceramicss, hydroapatite particles and its sintered product are hydroxyapatite crystalline phase.
Fig. 3 is to add hydroxyapatite overlong nanowire porous ceramicss (a) and hydroxyl phosphorus prepared by different content pore creating material
The digital photograph of the material (b) prepared after limestone particles sintering.As can be known from Fig. 3 with the increase of Content of Pore-forming Agents, gained hydroxyl
The pore distribution of base apatite overlong nanowire porous ceramicss it is more uniform, porosity gradually increases, nano wire ceramic structure
It is intact;And nano-particle base substrate structure collapses into powder body completely after sintering, it is impossible to obtain porous ceramicss.
Claims (10)
1. a kind of hydroxyapatite overlong nanowire porous ceramicss, it is characterised in that the hydroxyapatite overlong nanowire is more
Hole ceramics are prepared from as raw material by hydroxyapatite overlong nanowire.
2. hydroxyapatite overlong nanowire porous ceramicss according to claim 1, it is characterised in that the hydroxy-apatite
There is stone overlong nanowire porous ceramicss three-dimensional communication pore passage structure, channel diameter and porosity can adjust.
3. hydroxyapatite overlong nanowire porous ceramicss according to claim 1 and 2, it is characterised in that the hydroxyl
The length of apatite overlong nanowire is 30~1000 microns, a diameter of 5~100 nanometers.
4. the preparation method of the hydroxyapatite overlong nanowire porous ceramicss any one of a kind of claim 1-3, its
Be characterised by, hydroxyapatite overlong nanowire and pore creating material are uniformly mixed, the hydroxy-apatite is obtained Jing after molding, sintering
Stone overlong nanowire porous ceramicss.
5. preparation method according to claim 4, it is characterised in that the pore creating material is having of can decomposing under uniform temperature
Machine pore creating material or/and inorganic pore creating material, preferably palmitic acid.
6. the preparation method according to claim 4 or 5, it is characterised in that the hydroxyapatite overlong nanowire and make
The mass ratio of hole agent is 1:10~10:1.
7. the preparation method according to any one of claim 4-6, it is characterised in that it is described be shaped to tablet machine dry-pressing into
Type.
8. the preparation method according to claim 4-7, it is characterised in that the pressure of the molding is 1~50 MPa.
9. the preparation method according to any one of claim 4-8, it is characterised in that the atmosphere of the sintering is air gas
Atmosphere.
10. the preparation method according to any one of claim 4-9, it is characterised in that the temperature of the sintering is 800~
1600 DEG C, sintering time is more than 5 minutes, and the heating rate during sintering is 1~50 DEG C/min.
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CN107158805A (en) * | 2017-06-30 | 2017-09-15 | 宁波灏钻科技有限公司 | A kind of multifunctional compound ceramics filter core and preparation method thereof |
CN113416069A (en) * | 2021-02-01 | 2021-09-21 | 浙江农林大学 | Preparation method and application of hydroxyapatite nanowire sintered porous ceramic beads |
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