CN106542845B - Hydroxyapatite overlong nanowire porous ceramics and preparation method thereof - Google Patents
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Abstract
The present invention relates to hydroxyapatite overlong nanowire porous ceramics and preparation method thereof, the hydroxyapatite overlong nanowire porous ceramics is prepared as a raw material by hydroxyapatite overlong nanowire.The present invention prepares a kind of hydroxyapatite overlong nanowire porous ceramics with excellent biocompatibility, three-dimensional communication cellular structure and high porosity using hydroxyapatite overlong nanowire as raw material for the first time.
Description
Technical field
The present invention relates to a kind of hydroxyapatite overlong nanowire porous ceramics with three-dimensional communication cellular structure, specifically
It is related to having using hydroxyapatite overlong nanowire as raw material, using palmitic acid as pore creating material by forming, being sintered to prepare
The hydroxyapatite overlong nanowire porous ceramics of three-dimensional communication cellular structure, pore size and porosity can be added by pore creating material
Dosage regulates and controls.The invention belongs to ceramic material preparation fields.
Background technique
With excellent biocompatibility, three-dimensional communication cellular structure porous ceramics field of biomedicine have it is important
Application value can be used as bone impairment renovation material.Therefore, with excellent biocompatibility, three-dimensional communication cellular structure it is more
Hole ceramics receive more and more attention.
Up to the present, people have synthesized the hydroxyl with different porosities by a variety of different synthetic methods
The methods of apatite porous ceramics, including sol-gel, gel injection-moulding, freeze-dried and addition pore creating material.But for hydroxyl
The research that the pattern of base apatite influences prepared porous ceramics performance is also rarely reported.
Although current document has the synthetic method report of hydroxyapatite porous ceramics, in order to obtain high porosity
Hydroxyapatite porous ceramics, preparation method is more complex, and mostly using hydroxyapatite nanoparticle as raw material, institute
Porosity or/and the cellular structure for obtaining hydroxyapatite porous ceramics are undesirable.Using hydroxyapatite overlong nanowire as
Raw material prepares hydroxyapatite porous ceramics and has not been reported.
Summary of the invention
In view of the above-mentioned problems, the purpose of the present invention is to provide one kind to have excellent biocompatibility, three-dimensional communication duct
The hydroxyapatite overlong nanowire porous ceramics of structure and high porosity.
On the one hand, the present invention provides a kind of hydroxyapatite overlong nanowire porous ceramics, the hydroxyapatite is super
Long nano wire porous ceramics is prepared as a raw material by hydroxyapatite overlong nanowire.
The present invention for the first time using hydroxyapatite overlong nanowire as raw material prepare it is a kind of have excellent biocompatibility,
The hydroxyapatite overlong nanowire porous ceramics of three-dimensional communication cellular structure and high porosity.Compared to hydroxyapatite nano
There is high length-diameter ratio largely to make in the preparation process of porous ceramics even if joined for grain, hydroxyapatite overlong nanowire
Hole agent, due to the interaction between nano wire and nano wire, ceramic body will not collapse during the sintering process.
Preferably, the hydroxyapatite overlong nanowire porous ceramics has three-dimensional communication cellular structure, channel diameter
And adjustable porosity.
Preferably, the length of the hydroxyapatite overlong nanowire is 30~1000 microns, diameter is 5~100 nanometers.
On the other hand, the present invention provides the preparation method of above-mentioned hydroxyapatite overlong nanowire porous ceramics, comprising: will
Hydroxyapatite overlong nanowire and pore creating material uniformly mix, formed, be sintered after obtain the hydroxyapatite overlength nanometer
Line porous ceramics.
Preferably, the pore creating material be the organic pore-forming agents that can be decomposed at a certain temperature or with inorganic pore creating material, it is excellent
It is selected as palmitic acid.
Preferably, the mass ratio of the hydroxyapatite overlong nanowire and pore creating material is 10:1~1:10.
The present invention can also be by the content and size of control pore creating material, can be to the porous pottery of hydroxyapatite overlong nanowire
Porcelain pore size and porosity can be regulated and controled by pore creating material.
Preferably, described, to be shaped to tablet press machine dry-pressing formed.
Also, preferably, the molding pressure is 1~50MPa.
Preferably, the atmosphere of the sintering is air atmosphere.
Preferably, the temperature of the sintering is 800~1600 DEG C, sintering time is greater than 5 minutes.Also, preferably, the burning
Heating rate when knot is 1~50 DEG C/min, preferably 2~10 DEG C/min.
Hydroxyapatite provided by the invention with excellent biocompatibility, three-dimensional communication cellular structure and high porosity
Overlong nanowire porous ceramics, pore size and porosity can be regulated and controled by pore creating material.
Hydroxyapatite produced by the present invention with excellent biocompatibility, three-dimensional communication cellular structure and high porosity
Overlong nanowire porous ceramics can be applied to the multiple fields such as field of biomedicine.System of the present invention to extension porous ceramics
Standby and application has important scientific meaning and practical value.
Also, preparation process of the invention is simple and convenient to operate, the equipment for not needing complex and expensive is expected to realize industrialization.
Hydroxyapatite overlong nanowire of the present invention with excellent biocompatibility, three-dimensional communication cellular structure and high porosity
Porous ceramics has a good application prospect in multiple fields such as biomedicines.
Detailed description of the invention
Fig. 1 is that the scanning electron of the hydroxyapatite overlong nanowire porous ceramics of addition different content pore creating material preparation is aobvious
Micro- (SEM) photo；
Fig. 2 penetrates for the X of hydroxyapatite overlong nanowire and its porous ceramics, hydroapatite particles and its sintered product
Line diffraction (XRD) figure；
Fig. 3 is the hydroxyapatite overlong nanowire porous ceramics (upper row) and hydroxyl for adding the preparation of different content pore creating material
The digital photograph of the material (lower row) prepared after apatite particle 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, is not intended to limit the 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 decomposed etc. is used as pore creating material, is prepared by forming, being sintered with excellent biocompatibility, three-dimensional
The hydroxyapatite overlong nanowire porous ceramics of connected pore channel structure and high porosity.
Hydroxyapatite overlong nanowire porous ceramics prepared by the present invention has three-dimensional communication cellular structure, channel diameter
Porosity can be adjusted.
In the present invention, the length range of the hydroxyapatite overlong nanowire is 30 microns~1000 microns, nano wire
Diameter be 5 nanometers~100 nanometers.
Illustrate to following exemplary the preparation method of hydroxyapatite overlong nanowire porous ceramics provided by the invention.
Hydroxyapatite overlong nanowire of the present invention can be prepared using solvent-thermal method, can refer to document and patent report
Prepared by the method in road: Zhu Yingjie, Lu Bingqiang, Chen Feng, the non-ignitable hydroxyapatite paper and preparation method thereof of high-flexibility high temperature resistant,
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 methods, institute can also be used
As long as the hydroxyapatite overlong nanowire can be prepared with method is unlimited.
Hydroxyapatite overlong nanowire and pore creating material are uniformly mixed, at 800~1600 DEG C (preferably 1000 after forming
~1300 DEG C) under sintering be greater than 5 minutes (preferably 1 hour~5 hours), obtain the porous pottery of hydroxyapatite overlong nanowire
Porcelain.Specifically, weigh certain mass hydroxyapatite overlong nanowire and pore creating material (for example, palmitic acid, it is other it is organic,
Inorganic pore creating material etc.) it is uniformly mixed.And formed using certain molding mode (such as tablet press machine is dry-pressing formed, static pressure at
Type etc.).Using being burnt under conditions of certain sintering processing (Muffle furnace is normal pressure-sintered under such as air atmosphere) and experiment parameter
Knot.Preferably, heating rate can be 1 degrees celsius/minute~50 degrees celsius/minutes.Soaking time is greater than 5 minutes.Holding temperature
It is 800 degrees Celsius~1600 degrees Celsius.Being cooled to room temperature to temperature can be obtained with excellent biocompatibility, three-dimensional communication hole
The hydroxyapatite overlong nanowire porous ceramics of road structure and high porosity.
For forming and sintering, specifically, hydroxyapatite overlong nanowire is uniformly mixed with pore creating material, is put into tabletting
It in grinding tool (for example, stainless steel mould), forms, then transfers them in sintering furnace under a certain pressure, in certain heating
It is sintered under the conditions of rate, soaking time, holding temperature.
Molding can be used that tablet press machine is dry-pressing formed, and briquetting pressure can be 1~50MPa.Sintering can be used under air atmosphere often
Pressure sintering (pressureless sintering under air atmosphere), it should be understood that other moldings and sintering processing also can be used.Wherein, forming and sintering
When, briquetting pressure and sintering temperature are adjustable, and such as briquetting pressure 8MPa, sintering temperature is 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
It is selected with porosity, may be, for example, 1:10~10:1.The present invention, can by the usage amount and/or size of control pore creating material
With to the hydroxyapatite overlong nanowire porous ceramics pore size (channel diameter) and porosity regulate and control, more
Easily obtain the hydroxyapatite overlong nanowire with excellent biocompatibility, three-dimensional communication cellular structure and high porosity
Porous ceramics.For example, porosity can be increased when improving the usage amount of pore creating material；It, can be with when increasing the size of pore creating material
Increase pore size and porosity.Vice versa.In the present invention, a large amount of pore creating material can be used to obtain high porosity, example
If the mass ratio of hydroxyapatite overlong nanowire and pore creating material can be 1:10.When using a large amount of pore creating material, due to nanometer
Interaction between line and nano wire, ceramic body will not collapse during the sintering process.
The present invention has the advantage that
(1) preparation method is easy, the equipment for not needing complex and expensive, is expected to realize industrialization；
(2) hydroxy-apatite with excellent biocompatibility, three-dimensional communication cellular structure and high porosity can be prepared
Stone overlong nanowire porous ceramics；
(3) hydroxyapatite overlong nanowire porous ceramics obtained by being adjusted as the content of pore creating material and size
Pore size and porosity are without destroying its structure.
Hydroxyapatite overlong nanowire porous ceramics of the present invention is by hydroxyapatite overlong nanowire as former
Material is prepared, with excellent biocompatibility, three-dimensional communication cellular 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 ceramics, porosity by Archimedes's drainage.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only 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 hereafter exemplary specific value.
Production Example 1
At room temperature, respectively by 0.1760g CaCl2、0.3480g NaH2PO4, 0.700g NaOH be dissolved in 10mL deionization
In water.30min will be mixed under 9mL deionized water, 4mL methanol, 7mL oleic acid magnetic agitation, 10mL is successively added dropwise later
CaCl2Solution, 10mL NaOH solution, 10mLNaH2PO4Solution continues to stir 30min.Then this mixed solution is transferred to
In 100mL reaction kettle, sealing, after 180 DEG C of reactions for 24 hours, cooled to room temperature, product precipitates in ethanol, then with water, ethyl alcohol
It is washed repeatedly with hexamethylene repeatedly, until hydroxyapatite overlong nanowire water slurry pH close to 7.4, is protected at 4 DEG C later
It deposits.Finally obtain hydroxyapatite overlong nanowire.
Embodiment 1
At room temperature, by 100 milligrams of hydroxyapatite overlong nanowires and 350 milligrams of pore creating material palmitic acid (partial size 300-
700 microns) it is uniformly mixed, and be put into the stainless steel mould that diameter is 10 millimeters, depressing to diameter in 8MPa pressure is 10
The disk of millimeter, then the disk pressed is put into Muffle furnace normal pressure-sintered in air atmosphere, heating rate is 10 degrees Celsius/
Minute, and be sintered 4 hours under 1300 degrees Celsius, finally obtain with excellent biocompatibility, three-dimensional communication cellular structure and
The hydroxyapatite overlong nanowire porous ceramics of high porosity, as shown in I in Fig. 3 (a).Wherein gained hydroxyapatite overlength
The porosity of nano wire porous ceramics is 89%.
Embodiment 2
At room temperature, by 100 milligrams of hydroxyapatite overlong nanowires and 250 milligrams of pore creating material palmitic acid (partial size 300-
700 microns) it is uniformly mixed, and be put into the stainless steel mould that diameter is 10 millimeters, depressing to diameter in 8MPa pressure is 10
The disk of millimeter, then the disk pressed is put into Muffle furnace normal pressure-sintered in air atmosphere, heating rate is 10 degrees Celsius/
Minute, and be sintered 4 hours under 1300 degrees Celsius, finally obtain with excellent biocompatibility, three-dimensional communication cellular structure and
The hydroxyapatite overlong nanowire porous ceramics of high porosity, as shown in II in Fig. 3 (a).Wherein gained hydroxyapatite is super
The porosity of long nano wire porous ceramics is 84%.
Embodiment 3
At room temperature, by 100 milligrams of hydroxyapatite overlong nanowires and 150 milligrams of pore creating material palmitic acid (partial size 300-
700 microns) it is uniformly mixed, and be put into the stainless steel mould that diameter is 10 millimeters, depressing to diameter in 8MPa pressure is 10
The disk of millimeter, then the disk pressed is put into Muffle furnace normal pressure-sintered in air atmosphere, heating rate is 10 degrees Celsius/
Minute, and be sintered 4 hours under 1300 degrees Celsius, finally obtain with excellent biocompatibility, three-dimensional communication cellular structure and
The hydroxyapatite overlong nanowire porous ceramics of high porosity, as shown in III in Fig. 3 (a).Wherein gained hydroxyapatite is super
The porosity of long nano wire porous ceramics is 76%.
Comparative example 1
At room temperature, by 100 milligrams of hydroxyapatite nanoparticles and 350 milligrams of pore creating material palmitic acid (partial size 300-700
Micron) it is uniformly mixed, and be put into the stainless steel mould that diameter is 10 millimeters, depressing to diameter in 8MPa pressure is 10 millimeters
Disk, then the disk pressed is put into Muffle furnace normal pressure-sintered in air atmosphere, heating rate is 10 degree mins Celsius
Clock, and be sintered 4 hours under 1300 degrees Celsius.Blank structure collapses into powder completely, is unable to get porous ceramics, such as Fig. 3 (b)
Shown in middle I.
Comparative example 2
100 milligrams of hydroxyapatite nanoparticles and 250 milligrams of pore creating material palmitic acid (300-700 microns of partial size) are mixed
Uniformly, it and is put into the stainless steel mould that diameter is 10 millimeters, depresses to the disk that diameter is 10 millimeters in 8MPa pressure, then
The disk pressed is put into Muffle furnace normal pressure-sintered in air atmosphere, heating rate is 10 degrees celsius/minutes, and 1300
It is sintered 4 hours under degree Celsius.Blank structure collapses into powder completely, is unable to get porous ceramics, as shown in II in Fig. 3 (b).
Comparative example 3
100 milligrams of hydroxyapatite nanoparticles and 150 milligrams of pore creating material palmitic acid (300-700 microns of partial size) are mixed
Uniformly, it and is put into the stainless steel mould that diameter is 10 millimeters, depresses to the disk that diameter is 10 millimeters in 8MPa pressure, then
The disk pressed is put into Muffle furnace normal pressure-sintered in air atmosphere, heating rate is 10 degrees celsius/minutes, and 1300
It is sintered 4 hours under degree Celsius.Blank structure collapses into powder completely, is unable to get porous ceramics, as shown in III in Fig. 3 (b).
Fig. 1 is that the scanning electron of the hydroxyapatite overlong nanowire porous ceramics of addition different content pore creating material preparation is aobvious
Micro- (SEM) photo, wherein figure a1, a2, a3 are respectively pore creating material additive amount by under the ceramic different amplification of 150 milligrams of acquisitions
Electron scanning micrograph；B1, b2, b3 are respectively pore creating material additive amount by the different times magnifications of 250 milligrams of acquisition ceramics
Electron scanning micrograph under several；C1, c2, c3 are respectively that pore creating material additive amount is put by the ceramic difference of 350 milligrams of acquisitions
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 ceramics it is more uniform.In conjunction with the embodiments as Content of Pore-forming Agents increases known to 1-3, gained hydroxyl
The porosity of base apatite overlong nanowire porous ceramics is gradually increased.
Fig. 2 is hydroxyapatite overlong nanowire, hydroxyapatite overlong nanowire porous ceramics, 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 ceramics, hydroapatite particles and its sintered product are hydroxyapatite crystal phase.
Fig. 3 is the hydroxyapatite overlong nanowire porous ceramics (a) and hydroxyl phosphorus for adding the preparation of 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 ceramics it is more uniform, porosity is gradually increased, nano wire ceramic structure
It is intact；And structure collapses into powder to nano particle green body completely after sintering, is unable to get porous ceramics.
Claims (8)
1. a kind of hydroxyapatite overlong nanowire porous ceramics, which is characterized in that the hydroxyapatite overlong nanowire is more
Hole ceramics are prepared as a raw material by hydroxyapatite overlong nanowire, the length of the hydroxyapatite overlong nanowire
It is 5~100 nanometers for 30~1000 microns, diameter；
Hydroxyapatite overlong nanowire and pore creating material are uniformly mixed, to obtain the hydroxyapatite super after being formed, being sintered
Long nano wire porous ceramics；The mass ratio of the hydroxyapatite overlong nanowire and pore creating material is 1:10~2:3.
2. hydroxyapatite overlong nanowire porous ceramics according to claim 1, which is characterized in that the hydroxy-apatite
Stone overlong nanowire porous ceramics has three-dimensional communication cellular structure, and channel diameter and porosity can be adjusted.
3. hydroxyapatite overlong nanowire porous ceramics according to claim 1, which is characterized in that the pore creating material is
The organic pore-forming agents that can be decomposed under certain temperature or/and inorganic pore creating material.
4. hydroxyapatite overlong nanowire porous ceramics according to claim 3, which is characterized in that the pore creating material is
Palmitic acid.
5. hydroxyapatite overlong nanowire porous ceramics according to claim 1, which is characterized in that described to be shaped to press
Piece machine is dry-pressing formed.
6. hydroxyapatite overlong nanowire porous ceramics according to claim 1, which is characterized in that the molding pressure
Power is 1~50 MPa.
7. hydroxyapatite overlong nanowire porous ceramics according to claim 1, which is characterized in that the gas of the sintering
Atmosphere is air atmosphere.
8. hydroxyapatite overlong nanowire porous ceramics described in any one of -7 according to claim 1, which is characterized in that institute
The temperature for stating sintering is 800~1600 DEG C, and sintering time is greater than 5 minutes, and the heating rate when sintering is 1~50 DEG C/minute
Clock.
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