CN106007684A - Graphene alumina ceramic composite material and preparation method thereof - Google Patents
Graphene alumina ceramic composite material and preparation method thereof Download PDFInfo
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Abstract
Belonging to the field of biomedical material preparation, the invention in particular relates to a graphene alumina ceramic composite material and a preparation method thereof. Technically, the invention aims to provide a preparation method of a graphene alumina ceramic composite material, and the method includes the steps of: mixing 98-99.75%vol of alumina ceramic with 0.25-2%vol of graphene evenly, then pressing the mixture into a green body, performing sintering at 1450-1650DEG C, and then conducting cooling. The composite material prepared by the method provided by the invention has good matrix bending strength, fracture toughness and biocompatibility, and can be used for human body joints.
Description
Technical field
The invention belongs to the preparation field of bio-medical material, be specifically related to a kind of Graphene alumina ceramic composite material and system thereof
Preparation Method.
Background technology
The research of biomedical ceramics material as a multi-crossed disciplines field, along with material science, biology, medical science,
The breakthrough of nanotechnology, has obtained swift and violent development in the nearly more than ten years.In particular with Tissue Engineering Study and people
Material is deepened continuously with tissue and cell interaction understanding, to the requirement of the performance of biomedical ceramics material and function more
High, more diversified, and the design concept of material and the constantly bring forth new ideas range of application so that associated materials or the application of technology of preparing
Prospect is expanded further.Bioceramic material can be divided into biological living by the extent of reaction according to embedded material Yu bio-tissue
Property ceramic material and bio-inert ceramic materials.
Bio-inert ceramic materials refers mainly to stable chemical performance, good biocompatibility, occurs with tissue the most hardly
Reaction or react the least material, such as aluminium oxide ceramics, zirconia ceramics with tissue.The structure of this kind of ceramic material is all
More stable, the bonding force in molecule is relatively strong, and all has higher mechanical strength, wearability and chemical stability, mainly
Be made up of oxide ceramics, non-oxide ceramics etc., wherein with aluminum, magnesium, titanium, zirconium oxide applications the most extensive.Biological
The shortcoming of inert ceramic material is: chemical bond does not occur with bone, wrapped up by fibrous tissue in vivo or and osseous tissue between shape
The characteristic becoming fibrous tissue interface have impact on the application in bone defect healing of this material, there is fibrous tissue circle between bone and material
Face, hinders the combination of material and bone, surely can relax with bone the most afterwards, also affects the bone conductibility of material simultaneously, long
Phase is detained the defect in internal generation structure, makes osseous tissue produce the weakness in structure；Mechanical strength is the highest, wherein impact flexibility
The low greatest problem needing for ceramic material to overcome, and elastic modelling quantity is too high；Coefficient of friction is relatively big, and the rate of wear is bigger.
Aluminium oxide medical ceramic is a kind of bio-inert material, but aluminium oxide ceramics also has the characteristic of self, and aluminium oxide ceramics exists
Having good frictional behaviour in the transplanting in joint, these are all by the high intensity of itself, low-friction coefficient and good wear-resistant
Property determine, and the hydrophilic of alumina surface constitutes the hydration layer of very thin (＜ 5nm), and this layer absorbs water and formation helps
In the protecting film that biology is the most compatible.
But aluminium oxide medical ceramic remains the shortcoming the same with other biological inert ceramic material, the hydration layer of formation is led
Cause biocompatibility reduces.Many research worker and scholar have employed a series of method to solve problems.Such as: use
Many empty aluminium oxidies, make Porous form aluminium oxide ceramics, make osseous tissue grow into its space and make implant fix, it is ensured that plant
Enter the good combination of thing and tissue；The shortcoming of the method be reduce pottery mechanical strength, the intensity of porous alumina ceramic with
The increase of voidage and drastically reduce, be only used for low position of not bearing a heavy burden or bear a heavy burden.
Although aluminium oxide additive has a variety of, but in the world medical aluminium oxide ceramic additive there is is extra requirement, according to
These requirements and outcome research, only two kinds of modifier magnesium oxide and zirconium oxide can use.
There is article to point out, aluminium oxide and the powder that zirconium oxide mass ratio is 85 15 are mixed, obtain flat 600 DEG C of calcinings
All particle diameters are the meta tetragonal zircite of 9nm, and after 1425 DEG C of pressureless sintering, aluminium oxide and zirconic particle diameter are respectively
0.5 μm, 0.15 μm, the bending strength of this composite and fracture toughness have respectively reached 708MPa and 5.8MPa m1/2, but
It is that the zirconium oxide amount that the method adds is bigger, and has research to be easily generated low temperature aging, and the party after pointing out to add zirconium oxide
Method operation is many, more complicated.
Although the interpolation of magnesium oxide can not significantly improve the mechanical performance of aluminium oxide, but in sintering process the fusing point of magnesium oxide and
Softening point is high relative to aluminium oxide, therefore plays skeletal support effect at oxidation at high temperatures magnesium, it is possible to ensure the porcelain burnt out
Intensity.Therefore a lot of researchers both with the addition of magnesium oxide and also with the addition of zirconium oxide, referred to as magnesium oxide association when sintered alumina
Same Zirconia reinforced alumina, wherein the addition form of magnesium is magnesium hydroxide ion, and after calcining, zirconium oxide is stable tetragonal
Type, mass fraction is 0.03～0.10%, and magnesium oxide mass fraction is 0.5～2.5%.The product density using the method to prepare is little
In 4.0g/cm3, bending strength is 344.8MPa, but the oxidation magnesium amount that the method adds is the most more, and bending strength does not the most obtain
To improving.
Summary of the invention
For problems such as medical low, the poor biocompatibility of aluminium oxide ceramics toughness, the invention provides one and utilize Graphene to carry
High-alumina matrix bending strength and fracture toughness, the method for biocompatibility.
First technical problem to be solved by this invention is to provide the preparation method of a kind of Graphene alumina ceramic composite material.
The method comprises the following steps: 98～99.75%vol aluminium oxide ceramics and 0.25～2%vol Graphene is mixed, is pressed into life
Base, green compact cool down after 1450～1650 DEG C of sintering.
Preferably, in the preparation method of above-mentioned Graphene alumina ceramic composite material, the granularity of described aluminium oxide ceramics be 100～
200nm。
Preferably, in the preparation method of above-mentioned Graphene alumina ceramic composite material, the thickness of described Graphene is 6～8nm,
A diameter of 15～20um.
Preferably, in the preparation method of above-mentioned Graphene alumina ceramic composite material, described mixing uses ball mill mixing,
Rotating speed is 200～300r/min, and the time is 2～3h.
Preferably, in the preparation method of above-mentioned Graphene alumina ceramic composite material, described compacting uses cold isostatic press pressure
System, pressure is 200～300MPa.
Preferably, in the preparation method of above-mentioned Graphene alumina ceramic composite material, the relative density of described green compact be 45～
55%.
Preferably, in the preparation method of above-mentioned Graphene alumina ceramic composite material, described sintering time is 2～3h.
Preferably, in the preparation method of above-mentioned Graphene alumina ceramic composite material, it is warming up to sintering temperature with 5～10 DEG C/min
Degree.
Further, in the preparation method of above-mentioned Graphene alumina ceramic composite material, it is warming up to sintering temperature with 5 DEG C/min.
Preferably, in the preparation method of above-mentioned Graphene alumina ceramic composite material, it is passed through nitrogen hydrogen during described sintering or argon hydrogen mixes
Close gas.
Further, in the preparation method of above-mentioned Graphene alumina ceramic composite material, in described nitrogen hydrogen or argon hydrogen mixture
Nitrogen containing 95%vol or argon, the hydrogen of 5%vol.
Second technical problem to be solved by this invention is to provide the Graphene aluminium oxide ceramics composite wood that said method prepares
Material.
The inventive method has that step is simple and convenient to operate, raw material addition is few, low cost and other advantages.The inventive method adds
The Graphene added is few, and the Graphene mixing 0.75%vol just can make aluminium oxide bending strength increase by 60%, fracture toughness improve
70%；But to reach identical mechanical strength, aluminium oxide needs to mix CNT 10%vol, or mixes carborundum 10%vol,
Or mix zirconium oxide 15wt%.
The composite that the inventive method prepares have be difficult to aging, wearability good, bending strength, fracture toughness, biology
The advantages such as the compatibility is good.But traditional aluminium oxide add zirconia material at 100-400 DEG C life-time service especially at wet environment
Under may result in being remarkably decreased of mechanical property, be attended by its surface and surround and watch or the micro-crack of macroscopic view.
Accompanying drawing explanation
Fig. 1 pure alumina sinters out the scanning electron microscope (SEM) photograph of product
The scanning electron microscope (SEM) photograph of Fig. 2 composite of the present invention
Fig. 3 osteocyte is cytoactive test figure in without the culture fluid of blood plasma
Fig. 4 osteocyte is cytoactive test figure in the culture fluid containing blood plasma
Fig. 5 stem cell sinters out the growing state on product at pure alumina
Fig. 6 stem cell growing state on composite of the present invention
Specific embodiment
The preparation method of a kind of Graphene alumina ceramic composite material, comprises the following steps: by 98～99.75%vol aluminium oxidies
Ceramic powders and 0.25～2%vol unoxidized Graphene mix homogeneously in ball mill, put into after mixing in particular mold, adopt
Be pressed into the green compact of required given shape with cold isostatic pressure machine, green compact have been suppressed and have been placed into afterwards in pipe type sintering furnace
1450～1650 DEG C of sintered heat insulatings 2～3h, are passed through nitrogen hydrogen or argon hydrogen mixture, nitrogen or argon and ensure that sample is burning during sintering
Being in during knot in inert environments, hydrogen produces reaction with the remnant oxygen in environment thus ensures that during sintering, raw material is not oxidized, burns
By sintered body air cooling after having tied.
Preferably, during described mix homogeneously the rotating speed of ball mill be 200～300r/min, the time be 2～3h.
Preferably, the granularity of described aluminium oxide ceramics is 100～200nm.
Preferably, the thickness of described Graphene is 6～8nm, a diameter of 15～20um.
Preferably, the relative density of described green compact is 45～55%；Described relative density be compacting after with compacting before volume ratio.
Preferably, it is warming up to sintering temperature with 5～10 DEG C/min.Further, it is warming up to sintering temperature with 5 DEG C/min.
Preferably, nitrogen containing 95%vol or argon, the hydrogen of 5%vol in described nitrogen hydrogen or argon hydrogen mixture.
Present invention also offers the Graphene alumina ceramic composite material that said method prepares.
Embodiment 1
The mix homogeneously in ball mill by the alumina ceramic powder of 99.62%vol and the graphene film of 0.38%vol, the mixed powder time
2.5h, the granular size of alumina powder is 150nm, and Graphene thickness is 6～8nm, a diameter of 15～20um；Mixed powder work
After sequence completes, powder is placed among specific mould, uses cold isostatic pressure machine to be pressed into green compact, joint green compact relative
Density is 50%；Joint green compact have been suppressed to be placed in pipe type sintering furnace afterwards and have been sintered, and sintering temperature is 1650 DEG C, rise
Temperature speed is 5 DEG C/min, and temperature retention time is 2.5h；It is passed through nitrogen hydrogen during sintering sintering object is protected；Sinter it
After by sample air cooling, i.e. obtain composite of the present invention.
Carrying out MTT test, test result is: after three days, osteocyte survival rate on this composite is 0.63.
Embodiment 2
The mix homogeneously in ball mill by the alumina ceramic powder of 99.24%vol and the graphene film of 0.76%vol, the mixed powder time
2.5h, the granular size of alumina powder is 150nm, and Graphene thickness is 6～8nm, a diameter of 15～20um；Mixed powder work
After sequence completes, powder is placed among specific mould, uses cold isostatic pressure machine to be pressed into green compact, joint green compact relative
Density is 49%；Joint green compact have been suppressed to be placed in pipe type sintering furnace afterwards and have been sintered, and sintering temperature is 1645 DEG C, rise
Temperature speed is 5 DEG C/min, and temperature retention time is 2.5h；It is passed through nitrogen hydrogen during sintering sintering object is protected；Sinter it
After by sample air cooling, i.e. obtain composite of the present invention.
Carrying out MTT test, test result is: after three days, osteocyte survival rate on this composite is 0.64.
Embodiment 3
The mix homogeneously in ball mill by the alumina ceramic powder of 98.67%vol and the graphene film of 1.33%vol, the mixed powder time
2.3h, the granular size of alumina powder is 150nm, and Graphene thickness is 6～8nm, a diameter of 15～20um；Mixed powder work
After sequence completes, powder is placed among specific mould, uses cold isostatic pressure machine to be pressed into green compact, joint green compact relative
Density is 51%；Joint green compact have been suppressed to be placed in pipe type sintering furnace afterwards and have been sintered, and sintering temperature is 1645 DEG C, rise
Temperature speed is 5 DEG C/min, and temperature retention time is 2.3h；It is passed through nitrogen hydrogen during sintering sintering object is protected；Sinter it
After by sample air cooling, i.e. obtain composite of the present invention.
Carrying out MTT test, test result is: after three days, osteocyte survival rate on this composite is 0.65.
Table 1
Table 1 be pure alumina with aluminium oxide in mix different volumes Graphene after fire the composite obtained and under equal conditions survey
Fixed fracture toughness and intensity, as can be seen from Table 1, the fracture toughness of the composite that the inventive method prepares is with strong
Degree is substantially better than pure alumina.
Fig. 1 is the scanning electron microscope (SEM) photograph that pure alumina burns out product, and Fig. 2 is the scanning electron microscope (SEM) photograph of composite of the present invention, contrast
Fig. 1,2 analyses understand, substantially it can be observed how the composite crystal grain that the inventive method prepares becomes more under equal yardstick
Add uniformly.Fig. 3 is osteocyte cytoactive test figure in without the culture fluid of blood plasma, by this figure it can be seen that side of the present invention
Osteocyte survival rate on the composite that method prepares significantly improves.Fig. 4 is osteocyte cell in the culture fluid containing blood plasma
Active testing figure, by this figure it can be seen that increase in time, the cell on composite that the inventive method prepares
Increasing of survival rate is higher than pure alumina.Fig. 5 is that stem cell sinters out the growing state on product at pure alumina, by this figure
It can be seen that stem cell is to exist with the situation of point at alumina surface.Fig. 6 is that stem cell is on composite of the present invention
Growing state, by this figure it can be seen that stem cell is extended into lamellar on carrier, therefore deduce that prepared by the inventive method
Good than pure alumina of the biocompatibility of the composite obtained.
In summary it can be seen, the Graphene alumina ceramic composite material that the inventive method prepares has good intensity, breaks
Split the advantage such as toughness and biocompatibility, it is possible to meet the requirement as human synovial.So, the inventive method is medical treatment row
The human synovial in industry field provides a kind of preferably selection.
Claims (10)
1. the preparation method of a Graphene alumina ceramic composite material, it is characterised in that: comprise the following steps: by 98～
99.75%vol aluminium oxide ceramics and the mixing of 0.25～2%vol Graphene, be pressed into green compact, and green compact are at 1450～1650 DEG C of sintering
After cool down.
Preparation method the most according to claim 1, it is characterised in that: the granularity of described aluminium oxide ceramics is 100～200nm.
Preparation method the most according to claim 1, it is characterised in that: the thickness of described Graphene is 6～8nm, diameter
It is 15～20um.
Preparation method the most according to claim 1, it is characterised in that: described mixing uses ball mill mixing, and rotating speed is
200～300r/min, the time is 2～3h.
Preparation method the most according to claim 1, it is characterised in that: described compacting uses cold isostatic press compacting, pressure
Power is 200～300MPa.
Preparation method the most according to claim 1, it is characterised in that: the relative density of described green compact is 45～55%.
Preparation method the most according to claim 1, it is characterised in that: described sintering time is 2～3h.
Preparation method the most according to claim 1, it is characterised in that: it is warming up to sintering temperature with 5～10 DEG C/min；Excellent
Choosing, it is warming up to sintering temperature with 5 DEG C/min.
Preparation method the most according to claim 1, it is characterised in that: it is passed through nitrogen hydrogen or argon hydrogen mixture during described sintering；
Preferably, nitrogen containing 95%vol or argon, the hydrogen of 5%vol in described nitrogen hydrogen or argon hydrogen mixture.
10. the Graphene alumina ceramic composite material prepared by the preparation method described in any one of claim 1～9.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107311629A (en) * | 2017-07-24 | 2017-11-03 | 苏州宏久航空防热材料科技有限公司 | A kind of graphene/fullerene modification ceramic matric composite |
| CN107686365A (en) * | 2017-10-31 | 2018-02-13 | 湖南国盛石墨科技有限公司 | The application of spent FCC catalyst and using spent FCC catalyst as graphene/ceramic material of raw material and preparation method thereof |
| CN108640663A (en) * | 2018-08-15 | 2018-10-12 | 辽宁科技大学 | A kind of graphene/carbon SiClx enhancing alumina matrix composite and preparation method thereof |
| CN108975933A (en) * | 2018-09-18 | 2018-12-11 | 广东蓝狮医疗科技有限公司 | Wear-resistant aluminium oxide-zirconium oxide composite ceramics of a kind of graphite enhancing and preparation method thereof |
| CN110282959A (en) * | 2019-07-31 | 2019-09-27 | 深圳烯创先进材料研究院有限公司 | A kind of method of graphene Strengthening and Toughening aluminium oxide ceramics |
| CN112159242A (en) * | 2020-10-13 | 2021-01-01 | 齐鲁工业大学 | Graphene nanosheet based toughened alumina-titanium boride composite ceramic material and preparation method thereof |
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| CN108640663A (en) * | 2018-08-15 | 2018-10-12 | 辽宁科技大学 | A kind of graphene/carbon SiClx enhancing alumina matrix composite and preparation method thereof |
| CN108975933A (en) * | 2018-09-18 | 2018-12-11 | 广东蓝狮医疗科技有限公司 | Wear-resistant aluminium oxide-zirconium oxide composite ceramics of a kind of graphite enhancing and preparation method thereof |
| CN110282959A (en) * | 2019-07-31 | 2019-09-27 | 深圳烯创先进材料研究院有限公司 | A kind of method of graphene Strengthening and Toughening aluminium oxide ceramics |
| CN112159242A (en) * | 2020-10-13 | 2021-01-01 | 齐鲁工业大学 | Graphene nanosheet based toughened alumina-titanium boride composite ceramic material and preparation method thereof |
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