CN108727001A - A kind of zirconium dioxide toughening en plaque alumina-based composite ceramics and preparation method thereof - Google Patents
A kind of zirconium dioxide toughening en plaque alumina-based composite ceramics and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of zirconium dioxide toughening en plaque alumina-based composite ceramics and preparation method thereof.The invention discloses a kind of preparation methods of zirconium dioxide toughening en plaque alumina-based composite ceramics, including：Sequentially add the first dispersant, Al2O3Powder and ZrO2It is mixed after powder, the second dispersant is added, is sintered, obtains ZrO2Toughening en plaque Al2O3Base composite ceramic；First dispersant includes PAA and PEG；Second dispersant includes AMP and PEG.The preparation method is easy to operate, saves manufacturing cost, the Al in ZTA complex phase ceramic matrixes of the invention2O3Oriented growth occurs for crystal grain, with certain draw ratio, and it is in en plaque structure, the structure so that the probability of crack deflection and crackle bridge joint improves in fracture process, and then under the premise of not influencing ZTA complex phase ceramic hardness, the fracture toughness of ZTA complex phase ceramics significantly improves with intensity, solves existing ZTA complex phase ceramics matrix Al2O3Shape be etc. shaft-like pattern, the poor problem of toughness.
Description
Technical field
The present invention relates to technical field of composite materials more particularly to a kind of zirconium dioxide toughening en plaque alumina base are compound
Ceramics and preparation method thereof.
Background technology
Aluminium oxide (Al2O3) base ceramic material has that high temperature resistant, intensity be big, creep resistance, abrasion performance, good insulating, weight
Gently, the excellent characteristic such as anti-oxidant, is a kind of ideal structural ceramic material, and application is extremely wide.With the development of technology with
The expansion of application field, to Al2O3The performance requirement of base ceramic material also increasingly improves.
Al2O3Ceramics are also known as corundum, and Morse hardness is 9, extreme hardness.But due to Al2O3The higher brittleness of ceramics, makes it
Application range is restricted.In order to overcome this disadvantage, the security reliability during use is improved, Strengthening and Toughening is carried out to it
Processing is one of the important topic that professional scholar is always worked on for a long time.Currently, academia has proposed a variety of be directed to
Al2O3The method for toughening of base ceramic material, the more ripe and wide method of application have zirconium dioxide (ZrO2) toughening and fiber
Toughening, i.e., in Al2O3ZrO is added in matrix2Second phase forms ZrO2Toughening Al2O3Base composite ceramic (ZTA,
ZrO2toughened Al2O3)。
Currently, the matrix Al of ZTA complex phase ceramics2O3Shape be etc. shaft-like pattern, toughness is poor.
Invention content
The present invention provides a kind of zirconium dioxide toughening en plaque alumina-based composite ceramics and preparation method thereof, solve
Existing ZTA complex phase ceramics matrix Al2O3Shape be etc. shaft-like pattern, the poor technical problem of toughness.
Its specific technical solution is as follows：
The present invention provides one kind sequentially adding the first dispersant, aluminium oxide (Al2O3) powder and zirconium dioxide (ZrO2) powder
It is mixed after body, the second dispersant is added, is sintered, obtains ZrO2Toughening en plaque Al2O3Base composite ceramic；
First dispersant includes polyacrylic acid (PAA) and polyethylene glycol (PEG)；
Second dispersant includes 2-amino-2-methyl-1-propanol (AMP) and PEG.
Preferably, the Al2O3Diameter of particle is 80nm-200nm；
The ZrO2Diameter of particle is 40nm-200nm.
Preferably, the Al2O3Powder accounts for the Al2O3Powder and the ZrO2The 60vol.% of powder total content~
95vol.%, more preferably 80vol.%；
The ZrO2Powder accounts for the Al2O3Powder and the ZrO25vol.%~40vol.% of powder total content, more
Preferably 20vol.%.
Preferably, PAA, the PEG described in first dispersant account for the Al2O3Powder and ZrO2Powder total content
0.5wt.%~3wt.%, it is further preferred that PAA be 2wt.%, PEG 1wt.%.
Preferably, AMP, the PEG described in second dispersant account for the Al2O3Powder and ZrO2Powder total content
0.5wt.%~3wt.%, it is further preferred that AMP be 2wt.%, PEG 1.5wt.%.
Preferably, the sintering temperature is 1500 DEG C~1550 DEG C.
Preferably, described to obtain Al after the sintering2O3Before ceramics, further include：Heat preservation；
The time of the heat preservation is 0.5h~2h.
Preferably, the solvent of first dispersant and second dispersant is deionized water.
Specifically, ZrO2Toughening en plaque Al2O3Base composite ceramic preparation method is：
(1) the first dispersant is added in deionized water to being completely dissolved, Al is added2O3PH value is adjusted after powder, is added
ZrO2Powder obtains the first ZrO2Toughening Al2O3Base composite ceramic slurry；
(2) ZrO for obtaining step (1)2Toughening Al2O3After base composite ceramic slurry carries out ball milling, drying successively, obtain
First ZrO2Toughening Al2O3Base composite ceramic powder；
(3) the second dispersant is added in deionized water to being completely dissolved, the first ZrO of step (2) is added2Toughening Al2O3Base
Composite ceramic material adjusts pH value, obtains the 2nd ZrO2Toughening Al2O3Base composite ceramic slurry；
(4) ZrO for obtaining step (3)2Toughening Al2O3After base composite ceramic slurry carries out ball milling, drying, sieving successively,
Obtain the 2nd ZrO2Toughening Al2O3Base composite ceramic powder；
(5) to the 2nd ZrO2Toughening Al2O3Base composite ceramic powder carries out mist projection granulating, obtains the third ZrO of 80 mesh2Increase
Tough Al2O3Base composite ceramic powder, compression moulding obtain ZrO2Toughening Al2O3Base composite ceramic green compact；
(6) by step (5) ZrO2Toughening Al2O3Base composite ceramic green compact are sintered, and are obtained with en plaque Al2O3Crystal grain
ZrO2Toughening en plaque Al2O3Base composite ceramic.
Wherein, dissolving method is stirring and dissolving in step (1), and agitating device is magnetic agitation, whipping temp is 60 DEG C~
90 DEG C, preferably 80 DEG C, stir speed (S.S.) are 150rpm~250rpm, preferably 200rpm；
After adjusting pH value, ZrO is added2Before powder, further include：Stirring；Stirring is that supersonic synergic stirs, and agitating device is
Blade type stirrer；
ZrO is added2After powder, continues supersonic synergic and stir 20min~60min, preferably 30min；PH value is 10~11.
Step (2) ball milling is specifically, by the first ZrO2Toughening Al2O3Base composite ceramic slurry is placed in planetary ball mill tank,
Planetary ball mill 2h~4h is carried out using zirconia ball；
Drying device is rotation evaporimeter；
After drying, the first ZrO is obtained2Toughening Al2O3Before base composite ceramic powder, further include：To ZrO2Toughening Al2O3Base is multiple
It closes ceramic powder to be heated, removes organic matter, wherein heating temperature is 600 DEG C~650 DEG C, preferably 600 DEG C.
Dissolving method is stirring and dissolving in step (3), and agitating device is magnetic agitation, and whipping temp is 60 DEG C~90 DEG C,
Preferably 80 DEG C, stir speed (S.S.) is 150rpm~250rpm, preferably 200rpm；
After adjusting pH, continues supersonic synergic and stir 20min~60min, preferably 30min；
PH value is 9~11.
Step (4) ball milling is specially：By the 2nd ZrO2Toughening Al2O3Base composite ceramic slurry is placed in planetary ball mill tank,
Roll-type ball milling 6h~10h is carried out using zirconia ball；
Drying device is rotation evaporimeter.
The sieve of sieving is 160 mesh screens.
The spraying liquid of step (5) mist projection granulating is deionized water, can be to avoid introducing impurity using mist projection granulating；
The method of compression moulding is：Dry-pressing, cold isostatic compaction；
After compression moulding, ZrO is obtained2Toughening Al2O3Further include before base composite ceramic green compact：By 600 DEG C~650 DEG C, protect
Warm 1h~2h ventings organic matter.
The device of step (6) sintering is Muffle furnace, and the atmosphere of sintering is air atmosphere, and the pressure of sintering is normal pressure, sintering
Heating rate be 5 DEG C/min~15 DEG C/min.
The sintering method of the present invention is the sintering method of routine, simple for process, cost-effective.
The present invention also provides ZrO made from above-mentioned preparation method2Toughening en plaque Al2O3Base composite ceramic, the ZrO2
Toughening Al2O3The matrix Al of base composite ceramic2O3The shape of crystal grain is en plaque.
Preferably, the Al2O3The draw ratio of crystal grain is 1~5.
The present invention is by sequentially adding the first dispersant, Al2O3Powder and ZrO2It is mixed after powder, is added second point
Powder is sintered, and obtains ZrO2Toughening en plaque Al2O3Base composite ceramic, the preparation method are easy to operate, save preparation
Cost, in addition, the Al in the ZTA complex phase ceramic matrixes of the present invention2O3Oriented growth occurs for crystal grain, and draw ratio is 1~5, and is in plate
Laminated structure, which so that the probability of crack deflection and crackle bridge joint greatly improves in fracture process, and then is not influencing ZTA
Under the premise of complex phase ceramic hardness, fracture toughness and the intensity of ZTA complex phase ceramics significantly improve, and experimental data is it is found that ZTA
Complex phase ceramic Vickers hardness reaches as high as Hv=21 ± 1GPa, and fracture toughness reaches as high as KIC=8.60 ± 0.76MPam1/2。
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without having to pay creative labor, may be used also for those of ordinary skill in the art
To obtain other attached drawings according to these attached drawings.
Fig. 1 is the ZrO that the embodiment of the present invention 1 provides2Toughening en plaque Al2O3Base composite ceramic sample section scanning electron microscope
Figure；
Fig. 2 is the ZrO that the embodiment of the present invention 1 provides2Toughening en plaque Al2O3Base composite ceramic sample polishes Surface scan electricity
Mirror figure；
Fig. 3 is ZTA ceramics samples the first scanning electron microscope (SEM) photograph of burnishing surface that comparative example 1 of the present invention provides；
Fig. 4 is ZTA ceramics samples the second scanning electron microscope (SEM) photograph of burnishing surface that comparative example 1 of the present invention provides.
Specific implementation mode
An embodiment of the present invention provides a kind of zirconium dioxide toughening en plaque alumina-based composite ceramics and preparation method thereof,
It is difficult to form the ZTA complex phase ceramics of high-compactness, and ZTA complex phase ceramics for solving existing ZTA complex phase ceramics preparation method
Matrix Al2O3Shape be etc. shaft-like pattern, toughness is relatively low.
In order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below in conjunction with the present invention
Attached drawing in embodiment, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that disclosed below
Embodiment be only a part of the embodiment of the present invention, and not all embodiment.Based on the embodiments of the present invention, this field
All other embodiment that those of ordinary skill is obtained without making creative work, belongs to protection of the present invention
Range.
It is tried used in zirconium dioxide toughening en plaque alumina-based composite ceramics provided by the invention and preparation method thereof
Agent is available on the market.
Just a kind of zirconium dioxide toughening en plaque alumina-based composite ceramics provided by the present invention and its preparation side below
Method is described further.
Embodiment 1
(1) it takes a certain amount of deionized water to be placed in beaker, Al is added2O3Powder and ZrO2The polypropylene of powder quality 2%
Sour (PAA) and 1% polyethylene glycol (PEG), beaker is placed on magnetic stirring apparatus with 60~90 DEG C, 150~250rpm
Rotating speed is stirred to whole dissolvings；
(2) 20~40g Al are slowly added into step (1) acquired solution2O3Powder simultaneously adjusts solution ph to 10~11；
(3) beaker is placed in supersonic wave cleaning machine, while is stirred using blade type stirrer, supersonic synergic stirring
It is slowly added to 5~10g ZrO in the process2Powder.Continue supersonic synergic after addition and stir 30min, preparing becomes ZTA ceramic slurries
Material；
(4) the ZTA slurries of step (3) are placed in planetary ball mill tank, 2~4h of planetary ball mill is carried out using zirconia ball；
(5) the ZTA slurries after planetary ball mill are dried using Rotary Evaporators, the ZTA powders after drying are heated
To after 600 DEG C of venting organic matters, ZTA powders are obtained；
(6) it takes a certain amount of deionized water to be placed in beaker, the 2-amino-2-methyl-1-propanol of powder quality 2% is added
(AMP) and 1.5% PEG, by beaker be placed on magnetic stirring apparatus with the rotating speed of 60~90 DEG C, 150~250rpm stir to
All dissolvings；
(7) the ZTA powders obtained by 20~40g steps (5) are added into solution and adjust solution ph to 9~11, after will
Beaker is placed in supersonic wave cleaning machine, while stirring 30~60min using blade type stirrer supersonic synergic；
(8) the ZTA slurries of step (7) are placed in roll-type ball grinder, 6~10h of roll-type ball milling is carried out using zirconia ball；
(9) it utilizes rotary evaporating device to dry ZTA slurries, ZTA ceramic powders is made after crossing 160 mesh sieve；
(10) it uses deionized water to carry out mist projection granulating to ZTA powders obtained by step (9), obtains the ZTA powders of 80 mesh；
(11) powder passes through dry-pressing, cold isostatic compaction；
(13) green body after molding passes through 600 DEG C, keeps the temperature 1h venting organic matters, obtains green compact；
(14) green compact are placed in Muffle furnace, in normal pressure, air atmosphere, with the heating rate of 5~15 DEG C/min,
It is sintered at 1500~1550 DEG C, keeps the temperature 0.5~2h, obtain ZrO2Toughening Al2O3Base composite ceramic.
As depicted in figs. 1 and 2, the ZrO2Toughening en plaque Al2O3Base composite ceramic compact structure, and matrix Al2O3Crystal grain
For en plaque, relative density is higher than 99%, and Vickers hardness is up to Hv=21 ± 1GPa, and fracture toughness is up to KIC=8.60 ±
0.76MPa·m1/2。
Comparative example 1
(1) it takes a certain amount of deionized water to be placed in beaker, Al is added2O3Powder and ZrO2The poly- second two of powder quality 2%
Beaker is placed on magnetic stirring apparatus and is stirred to whole dissolvings with the rotating speed of 80 DEG C, 200rpm by alcohol (PEG)；
(2) 20g Al are slowly added into step (1) acquired solution2O3Powder simultaneously adjusts solution ph to 10~11；
(3) beaker is placed in supersonic wave cleaning machine, while is stirred using blade type stirrer, supersonic synergic stirring
It is slowly added to 5g ZrO in the process2Powder.Continue supersonic synergic after addition and stir 30min, preparing becomes ZTA ceramic slurries；
(4) the ZTA slurries of step (3) are placed in planetary ball mill tank, 2~4h of planetary ball mill is carried out using zirconia ball；
(5) ZTA ceramics are made after crossing 160 mesh sieve in the ZTA slurries for utilizing rotary evaporating device drying steps (4) to be obtained
Powder；
(6) powder passes through dry-pressing, cold isostatic compaction；
(7) green body after molding passes through 600 DEG C, keeps the temperature 1h venting organic matters, obtains green compact；
(8) green compact are placed in Muffle furnace, in normal pressure, air atmosphere, with the heating rate of 5~15 DEG C/min,
It is sintered at 1500~1550 DEG C, keeps the temperature 0.5~2h, obtain ZTA ceramics samples.
As shown in Figure 3 and Figure 4, ZTA ceramics samples compact structure, Vickers hardness are up to Hv=20 ± 1GPa, Al2O3It is brilliant
Grain for etc. shaft-like, fracture toughness be up to KIC=4.21 ± 0.68MPam1/2。
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to before
Stating embodiment, invention is explained in detail, it will be understood by those of ordinary skill in the art that：It still can be to preceding
The technical solution recorded in each embodiment is stated to modify or equivalent replacement of some of the technical features；And these
Modification or replacement, the spirit and scope for various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of preparation method of zirconium dioxide toughening en plaque alumina-based composite ceramics, which is characterized in that including following step
Suddenly：
Sequentially add the first dispersant, aluminium oxide (Al2O3) powder and zirconium dioxide (ZrO2) mixed after powder, it is added the
Two dispersants, are sintered, and obtain ZrO2Toughening en plaque Al2O3Base composite ceramic；
First dispersant includes polyacrylic acid (PAA) and polyethylene glycol (PEG)；
Second dispersant includes 2-amino-2-methyl-1-propanol (AMP) and PEG.
2. preparation method according to claim 1, which is characterized in that the Al2O3Diameter of particle is 80nm-200nm；
The ZrO2Diameter of particle is 40nm-200nm.
3. preparation method according to claim 1, which is characterized in that the Al2O3Powder accounts for the Al2O3Powder and described
ZrO260vol.%~95vol.% of powder total content；
The ZrO2Powder accounts for the Al2O3Powder and the ZrO25vol.%~40vol.% of powder total content.
4. preparation method according to claim 1, which is characterized in that PAA, the PEG described in first dispersant
Account for the Al2O3Powder and ZrO20.5wt.%~3wt.% of powder total content.
5. preparation method according to claim 1, which is characterized in that AMP, the PEG described in second dispersant
Account for the Al2O3Powder and ZrO20.5wt.%~3wt.% of powder total content.
6. preparation method according to claim 1, which is characterized in that the sintering temperature is 1500 DEG C~1550 DEG C.
7. preparation method according to claim 1, which is characterized in that described to obtain ZrO after the sintering2Toughening
Al2O3Before base composite ceramic, further include：Heat preservation；
The time of the heat preservation is 0.5h~2h.
8. preparation method according to claim 1, which is characterized in that first dispersant and second dispersant
Solvent is deionized water.
9. ZrO made from the preparation method described in claim 1 to claim 8 any one2Toughening en plaque Al2O3Base is multiple
Close ceramics, which is characterized in that the ZrO2Toughening Al2O3The matrix Al of base composite ceramic2O3The shape of crystal grain is en plaque.
10. ZrO according to claim 92Toughening en plaque Al2O3Base composite ceramic, which is characterized in that the Al2O3It is brilliant
The draw ratio of grain is 1~5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109320272A (en) * | 2018-12-10 | 2019-02-12 | 新沂北美高科耐火材料有限公司 | A kind of novel environment friendly chrome corundum brick and its production technology |
| CN111410518A (en) * | 2020-05-15 | 2020-07-14 | 郑州中瓷科技有限公司 | Grain-graded zirconia toughened alumina ceramic substrate and preparation process thereof |
| TWI716271B (en) * | 2020-02-03 | 2021-01-11 | 中國鋼鐵股份有限公司 | Ceramic green body and method for fabricating the same |
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