CN107056316A - A kind of preparation method of high length-diameter ratio alumina whisker Strengthening and Toughening Ce TZP complex phase ceramics - Google Patents
A kind of preparation method of high length-diameter ratio alumina whisker Strengthening and Toughening Ce TZP complex phase ceramics Download PDFInfo
- Publication number
- CN107056316A CN107056316A CN201710471191.3A CN201710471191A CN107056316A CN 107056316 A CN107056316 A CN 107056316A CN 201710471191 A CN201710471191 A CN 201710471191A CN 107056316 A CN107056316 A CN 107056316A
- Authority
- CN
- China
- Prior art keywords
- complex phase
- tzp
- whisker
- slurry
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C04B35/803—
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5276—Whiskers, spindles, needles or pins
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a kind of preparation method of high length-diameter ratio alumina whisker Strengthening and Toughening Ce TZP complex phase ceramics, including：After water, polyethylene glycol and the propyl alcohol of 2 amino, 2 methyl 1 are mixed, regulation pH value is to 10~11, then and Al2O3Whisker is mixed, and under conditions of ultrasound and stirring, ball milling obtains Al2O3Whisker slurry；Under conditions of ultrasound and stirring, by Ce TZP powders and Al2O3Whisker slurry is mixed, and obtains complex phase mixed slurry；By complex phase mixed slurry ball milling, regulation pH value to 10~11, then be stirred successively, dried and screened, obtain composite ceramic material；By composite ceramic material dry-pressing, cold isostatic compaction, green compact are obtained；By green sintering, Al is obtained2O3Whiskers high-toughenedization Ce TZP complex phase ceramics.This method realizes the complete densification of complex phase ceramic by pressureless sintering, makes it have fine and close and uniform microstructure, and higher intensity and toughness.
Description
Technical field
The present invention relates to zirconium oxide complex phase ceramic technical field, more particularly to a kind of high length-diameter ratio alumina whisker Strengthening and Toughening
The preparation method of Ce-TZP complex phase ceramics.
Background technology
Tetragonal polycrystal zirconia ceramics (TZP) are due to its excellent mechanical property, chemical stability, biocompatibility
Deng being widely used as biologic implant material.
Pure zirconia can exist with monoclinic phase at normal temperatures, therefore need to pass through doped yttrium oxide (Y2O3), cerium oxide
(CeO2), magnesia (MgO) etc. make it stable in Tetragonal.Relative to Y2O3Stabilizing zirconia (Y-TZP), CeO2Stable oxidation
Zirconium (Ce-TZP) has higher toughness and more preferable low temperature aging resistance, therefore is more suitable for answering for biomedical sector
With.
Prior art is by introducing the aluminum oxide (Al with high intensity, high elastic modulus2O3) whisker, can further it carry
The intensity and toughness of high Ce-TZP materials, have a extensive future.As patent publication No. 105622075A discloses a kind of sapphire
Whisker and ZrO2Coordination plasticizing Al2O3The preparation method of ceramics, Al2O3Whisker and zirconium oxide are used simultaneously multiple with toughened aluminum oxide
Phase ceramics, but described by the patent, it is known that its process for dispersing does not obtain improvement, and whisker Ball-milling Time is long, and draw ratio is
Serious reduction, therefore inhibitory action reduction of the whisker to matrix material densification process, crystal whisker toughened meaning are not deposited again
.Therefore, the Al of high-compactness how is obtained2O3Whiskers high-toughenedization Ce-TZP composite ceramicses, as the bottleneck institute for preparing the material
.
The content of the invention
In view of this, it is an object of the invention to provide a kind of high length-diameter ratio alumina whisker Strengthening and Toughening Ce-TZP complex phases pottery
The preparation method of porcelain, high length-diameter ratio alumina whisker Strengthening and Toughening Ce-TZP complex phase ceramics consistency prepared by this method is high, micro-
Even structure, and then with higher intensity and toughness.
The invention provides a kind of preparation method of high length-diameter ratio alumina whisker Strengthening and Toughening Ce-TZP complex phase ceramics, including
Following steps：
A) after water, polyethylene glycol and 2-amino-2-methyl-1-propanol being mixed, regulation pH value to 10~11, Ran Houhe
Al2O3Whisker is mixed, and under conditions of ultrasound and stirring, ball milling obtains the Al of different draw ratios2O3Whisker slurry；
B) under conditions of ultrasound and stirring, by the Al2O3Whisker slurry and the mixing of Ce-TZP powders, obtain complex phase and mix
Close slurry；
C) by the complex phase mixed slurry ball milling, regulation pH value is to 10~11, then carries out blade stirring, drying and mistake successively
Sieve, obtains composite ceramic material；
D) composite ceramic material is heated after dry-pressing, cold isostatic compaction, obtains green compact；
E) by the green sintering, high length-diameter ratio Al is obtained2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics.
Preferably, Al in the step a)2O3The initial draw ratio of whisker is 42~78.
Preferably, Al in the step a)2O3Whisker account for solid powder content in the complex phase mixed slurry 5~
15vol%.
Preferably, the solid content of complex phase mixed slurry is 20~30vol% in the step b)；Ce-TZP powders account for described
85~95vol% of solid powder content in complex phase mixed slurry.
Preferably, the rotating speed of complex phase mixed slurry ball milling is 50~70rpm in the step c)；The complex phase slurry ball milling
Time be 10~20min.
Preferably, the temperature of blade stirring is 55~65 DEG C in the step c)；The time of blade stirring is 9~11h；Oar
The speed of leaf stirring is 180~220rpm.
Preferably, the temperature of heating is 550~650 DEG C in the step d)；The time of the heating is 0.5~1.2h.
Preferably, the temperature of sintering is 1400~1450 DEG C in the step e)；The time of sintering is 0.5~1h；Sintering
Atmosphere be air atmosphere；The pressure of sintering is normal pressure.
The invention provides the preparation method of high length-diameter ratio alumina whisker Strengthening and Toughening Ce-TZP complex phase ceramics, including it is following
Step：A) will be after water, polyethylene glycol and 2-amino-2-methyl-1-propanol mix, then and Al regulation pH value is to 10~11,2O3
Whisker is mixed, and under conditions of ultrasound and stirring, ball milling obtains the Al of different draw ratios2O3Whisker slurry；B) in ultrasound and stirring
Under conditions of, by the Al2O3Whisker slurry and the mixing of Ce-TZP powders, obtain complex phase mixed slurry；C) complex phase is mixed
Slurry ball milling, regulation pH value is to 10~11, then carries out blade stirring, dried and screened successively, obtains composite ceramic material；D) will
The composite ceramic material is heated after dry-pressing, cold isostatic compaction, obtains green compact；E) by the green sintering, high length is obtained
Compare Al in footpath2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics.This method is with CeO2Stabilizing zirconia (Ce-TZP) powder is raw material,
Al2O3Whisker mends tough phase for enhancing, by Al2O3The decentralized processing of whisker and slurry, then be sintered, you can realize
Al2O3The complete densification of whiskers high-toughenedization Ce-TZP complex phase ceramics, and uniform microstructure, with higher intensity and toughness.
Test result indicates that：High length-diameter ratio Al2O3The relative density of whiskers high-toughenedization Ce-TZP complex phase ceramics is higher than 99%, high length-diameter ratio
Al2O3The fracture toughness of whiskers high-toughenedization Ce-TZP complex phase ceramics is 10~15MPam1/2, bending strength be 500~
1000MPa。
Brief description of the drawings
Fig. 1 is that the embodiment of the present invention 1 prepares high length-diameter ratio Al2O3The technological process of whiskers high-toughenedization Ce-TZP complex phase ceramics
Figure；
Fig. 2 is the Al prepared by the embodiment of the present invention 12O3The ESEM of whiskers high-toughenedization Ce-TZP complex phase ceramic sections
Figure；
Fig. 3 is the Al prepared by comparative example 1 of the present invention2O3The ESEM of whiskers high-toughenedization Ce-TZP complex phase ceramic sections
Figure；
Fig. 4 is the Al prepared by comparative example 2 of the present invention2O3The ESEM of whiskers high-toughenedization Ce-TZP complex phase ceramic sections
Figure.
Embodiment
The invention provides a kind of preparation method of high length-diameter ratio alumina whisker Strengthening and Toughening Ce-TZP complex phase ceramics, including
Following steps：
A) after water, polyethylene glycol and 2-amino-2-methyl-1-propanol being mixed, regulation pH value to 10~11, Ran Houhe
Al2O3Whisker is mixed, and under conditions of ultrasound and stirring, ball milling obtains the Al of different draw ratios2O3Whisker slurry；
B) under conditions of ultrasound and stirring, by the Al2O3Whisker slurry and the mixing of Ce-TZP powders, obtain complex phase and mix
Close slurry；
C) by the complex phase mixed slurry ball milling, regulation pH value is to 10~11, then carries out blade stirring, drying and mistake successively
Sieve, obtains composite ceramic material；
D) composite ceramic material is heated after dry-pressing, cold isostatic compaction, obtains green compact；
E) by the green sintering, high length-diameter ratio Al is obtained2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics.
This method is with CeO2Stabilizing zirconia (Ce-TZP) powder is raw material, Al2O3Whisker mends tough phase for enhancing, by right
Al2O3The decentralized processing of whisker and slurry, then be sintered, you can realize high length-diameter ratio Al2O3Whiskers high-toughenedization Ce-TZP is answered
The complete densification of phase ceramics, makes it have higher intensity and toughness.
After the present invention mixes water, polyethylene glycol and 2-amino-2-methyl-1-propanol, regulation pH value to 10~11, then
And Al2O3Whisker is mixed, and under conditions of ultrasound and stirring, ball milling obtains the Al of different draw ratios2O3Whisker slurry.The present invention
It is preferred that water and polyethylene glycol are first mixed, then mixed with 2-amino-2-methyl-1-propanol.The present invention is preferably by water and poly- second two
Alcohol is mixed on magnetic stirring apparatus well known to those skilled in the art；The temperature of water and the polyethylene glycol mixing is preferred
For 55~65 DEG C, more preferably 58~63 DEG C；The time of water and the polyethylene glycol mixing is preferably 15~25min, more preferably
For 18~23min；Stir speed (S.S.) is preferably 180~220rpm during water and the polyethylene glycol mixing, more preferably 190~
210rpm.The addition of the polyethylene glycol preferably accounts for the 1.8~2.2% of solid powder quality, and the solid powder includes
Al2O3Whisker and CeO2Oxide-stabilizing zirconia powder (Ce-TZP powders)；In a particular embodiment of the present invention, preferably 60mL is gone
Ionized water is placed in beaker, adds the polyethylene glycol (PEG) for accounting for solid powder quality 2% in whisker slurry, beaker is placed in into magnetic
20min is stirred with 60 DEG C, 200rpm rotating speed on power agitating device.The present invention by water and polyethylene glycol it is well mixed after again and 2-
Amino-2-methyl -1- propyl alcohol is mixed；The addition of the 2-amino-2-methyl-1-propanol preferably accounts for solid powder quality
0.13~0.18%.
The present invention adds Al under conditions of supersonic synergic stirring2O3Whisker, obtains mixture；Add Al2O3It is excellent after whisker
Choosing continues supersonic synergic stirring 28~34min, more preferably 30min.Al2O3The initial draw ratio of whisker is preferably 42~78.Institute
State Al2O3Whisker accounts for 5~15vol% of solid powder content in the complex phase mixed slurry.
The present invention carries out the ball milling of mixture preferably in ball grinder well known to those skilled in the art.The zirconium oxide is excellent
Choosing uses a diameter of 5mm zirconium oxide balls.The rotating speed of the mixture ball milling is preferably 50~70rpm；The mixture ball
The time of mill is preferably 0.5~4h.The Al of the different draw ratios2O3Al in whisker slurry2O3The draw ratio of whisker is 5~35.
Mixture is preferably placed in after ball milling terminates in ball grinder in supersonic wave cleaning machine by the present invention again continues ultrasound, association
Same blade type stirrer, obtains the Al of different draw ratios2O3Whisker slurry；Supersonic synergic oar blade type stirring time be preferably
28~32min, more preferably supersonic synergic oar blade type stir 30min.
The present invention is under conditions of ultrasound and stirring, by the Al2O3Whisker slurry and the mixing of Ce-TZP powders, are answered
Mix slurry.In the present invention, solid content is preferably 20~30vol% in the complex phase mixed slurry；The Ce-TZP powder
The addition of body preferably accounts for 85~95vol% of solid powder content in whisker slurry, more preferably 87~92vol%, optimal
Elect 90vol% as.
Ce-TZP powders are preferably slowly added to after finishing by the present invention, and obtained mixture is continued into supersonic synergic stirring 27
~34min, more preferably 29~32min.
Obtain after complex phase mixed slurry, the complex phase mixed slurry ball milling is adjusted pH value to 10~11 by the present invention, then according to
Secondary progress blade stirring, dried and screened, obtain composite ceramic material.The present invention is preferably by complex phase mixed slurry and diameter 5mm
Zirconium oxide balls ball milling；The rotating speed of ball milling is preferably 50~70rpm after complex phase mixed slurry and the zirconium oxide mixing；It is described
The time of ball milling is preferably 10~20min after complex phase mixed slurry and zirconium oxide mixing, more preferably 12~18min, most preferably
For 15min.The present invention preferably will be placed in supersonic wave cleaning machine again after complex phase mixed slurry and diameter 5mm zirconium oxide balls ball milling
In, while stirring 27~34min using blade type stirrer supersonic synergic.Adjust after pH value preferably in those skilled in the art
It is stirred on well known magnetic stirring apparatus；The temperature of the blade stirring is preferably 55~65 DEG C；The time of blade stirring
Preferably 9~11h；The speed of blade stirring is preferably 180~220rpm.Done present invention preferably employs rotary evaporating device
It is dry.Sieved present invention preferably employs 100 mesh sieves.
Obtain after composite ceramic material, the body formed rear heating of the composite ceramic is obtained green compact by the present invention.The present invention
It is preferred to use dry-pressing or cold isostatic compaction mode is body formed by composite ceramic.In the present invention, the temperature of the heating is excellent
Elect 550~650 DEG C, more preferably 600 DEG C as；The time of the heating is preferably 1~2h, more preferably 1h.The present invention passes through
Heating excludes organic matter in green compact.
Obtain after green compact, the green sintering is obtained high length-diameter ratio Al by the present invention2O3Whiskers high-toughenedization Ce-TZP complex phases
Ceramics, i.e. tetragonal phase zirconium oxide ceramics.The present invention is preferably sintered in Muffle furnace well known to those skilled in the art.At this
In invention, the temperature of the sintering is preferably 1400~1450 DEG C；The time of the sintering is preferably 0.5~1h；The sintering
Atmosphere be preferably air atmosphere；The pressure of sintering is preferably normal pressure.The high length-diameter ratio Al2O3Whiskers high-toughenedization Ce-TZP is answered
Al in phase ceramics2O3The draw ratio of whisker is 5~35.
The invention provides a kind of high length-diameter ratio Al2O3The preparation method of whiskers high-toughenedization Ce-TZP complex phase ceramics, including with
Lower step：A) after water, polyethylene glycol and 2-amino-2-methyl-1-propanol being mixed, regulation pH value to 10~11, Ran Houhe
Al2O3Whisker is mixed, and under conditions of ultrasound and stirring, ball milling obtains the Al of different draw ratios2O3Whisker slurry；B) in ultrasound
Under conditions of stirring, by the Al2O3Whisker slurry and the mixing of Ce-TZP powders, obtain complex phase mixed slurry；C) will be described multiple
Slurry ball milling is mixed, regulation pH value is to 10~11, then carries out blade stirring, dried and screened successively, obtains composite ceramic
Body；D) composite ceramic material is heated after dry-pressing, cold isostatic compaction, obtains green compact；E) by the green sintering, obtain
To high length-diameter ratio Al2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics.This method is with CeO2Stabilizing zirconia (Ce-TZP) powder is original
Material, Al2O3Whisker mends tough phase for enhancing, by Al2O3The decentralized processing of whisker and slurry, then be sintered, you can realize
High length-diameter ratio Al2O3The complete densification of whiskers high-toughenedization Ce-TZP complex phase ceramics, makes it have higher intensity and toughness.It is real
Result is tested to show：High length-diameter ratio Al2O3The relative density of whiskers high-toughenedization Ce-TZP complex phase ceramics is higher than 99%, high length-diameter ratio
Al2O3The fracture toughness of whiskers high-toughenedization Ce-TZP complex phase ceramics is 10~15MPam1/2, bending strength be 500~
1000MPa。
In order to further illustrate the present invention, a kind of high length-diameter ratio Al provided with reference to embodiment the present invention2O3Whisker
The preparation method of Strengthening and Toughening Ce-TZP complex phase ceramics is described in detail, but can not be interpreted as them to present invention protection model
The restriction enclosed.
Embodiment 1
Referring to Fig. 1, Fig. 1 is the process chart that the embodiment of the present invention 1 prepares tetragonal phase zirconium oxide ceramics：
(1) take 60mL deionized waters to be placed in beaker, add the polyethylene glycol (PEG) of powder quality 2%, beaker is placed in
20min is stirred with 60 DEG C, 200rpm rotating speed on magnetic stirring apparatus；
(2) 2-amino-2-methyl-1-propanol (AMP-95) of powder quality 0.15%, regulation solution ph to 10 are added
~11；
(3) beaker is placed in supersonic wave cleaning machine, while stirred using blade type stirrer, supersonic synergic stirring
During be slowly added to Al2O3Whisker, total addition of solid powder is configured according to slurry solid content 25vol%, wherein Al2O3
Whisker accounts for the 10vol% of solid powder total amount, adds after whisker and continues supersonic synergic stirring 30min；
(4) by the Al of step (3)2O3Whisker slurry takes out, and is placed in ball grinder, using 5mm zirconium oxide balls, utilizes rolling
Formula ball mill is with the slow 0.5~4h of ball milling of 50~70rpm rotating speed；
(5) by the Al after ball milling2O3Whisker slurry is placed in beaker, and beaker is placed in supersonic wave cleaning machine, while using oar
Leaf formula agitating device, supersonic synergic stirring 30min；
(6) continue to keep supersonic synergic stirring, to Al2O3Solid powder total amount is slowly added in whisker slurry
90vol% Ce-TZP powders, plus continue supersonic synergic stirring complex phase mixed slurry 30min after the completion of powder；
(7) the complex phase mixed slurry of step (6) is taken out, is placed in ball grinder, using 5mm zirconium oxide balls, utilizes rolling
Formula ball mill is with 50~70rpm rotating speed low speed ball milling 15min；
(8) the complex phase slurry after ball milling is replaced in beaker, beaker is placed in supersonic wave cleaning machine, while using oar
Leaf formula agitating device supersonic synergic stirs 30min；
(9) complex phase slurry pH value is adjusted to 10~11；
(10) beaker is placed on magnetic stirring apparatus and 10h is stirred with 60 DEG C, 200rpm rotating speed；
(11) complex phase slurry is dried using rotary evaporating device, crosses and Al is made after 100 mesh sieves2O3Whisker is combined Ce-TZP potteries
Porcelain powder；
(12) powder passes through dry-pressing, cold isostatic compaction；
(13) base substrate after being molded passes through 600 DEG C, is incubated 1h venting organic matters, obtains green compact；
(14) green compact are placed in Muffle furnace, in normal pressure, air atmosphere, with 10 DEG C/min heating rate by furnace temperature liter
To 1000 DEG C, heated up afterwards with 5 DEG C/min heating rate, being incubated 30min at 1400~1450 DEG C is sintered, and obtains densification
High length-diameter ratio Al2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics, i.e. tetragonal phase zirconium oxide ceramics.
The high length-diameter ratio Al that the present invention is prepared to embodiment 12O3Whiskers high-toughenedization Ce-TZP complex phase ceramics progress consistency,
The test of hardness, fracture toughness and bending strength, test result is：High length-diameter ratio Al prepared by embodiment 12O3Whiskers high-toughenedization
The relative density of Ce-TZP complex phase ceramics is higher than 99%, and fracture toughness is 10~15MPam1/2, bending strength be 500~
1000MPa。
By the Al prepared by the embodiment of the present invention 12O3Whiskers high-toughenedization Ce-TZP complex phase ceramic sections are scanned electronic display
Micro mirror is observed, as a result as shown in Fig. 2 Fig. 2 is the Al prepared by the embodiment of the present invention 12O3Whiskers high-toughenedization Ce-TZP complex phase ceramics
The scanning electron microscope (SEM) photograph of section.The Al that Fig. 2 displays are prepared using this method2O3Whiskers high-toughenedization Ce-TZP complex phase ceramic sections are micro-
Even structure, whisker is well dispersed, no significant defect, and fine and close.
Comparative example 1
Al is prepared according to the method for embodiment 12O3Whisker is combined Ce-TZP ceramic powders, as different from Example 1, step
Suddenly (4)~(6) use following technique, and omit step (7).
(4) continue to keep supersonic synergic stirring, to Al2O3Solid powder total amount is slowly added in whisker slurry
90vol% Ce-TZP powders, plus continue supersonic synergic stirring complex phase mixed slurry 30min after the completion of powder；
(5) by the Al of step (4)2O3Whisker Ce-TZP complex phases mixed slurry takes out, and is placed in ball grinder, is aoxidized using 5mm
Zirconium abrading-ball, using roll-type ball mill with the slow 0.5~4h of ball milling of 50~70rpm rotating speed；
(6) by the Al after ball milling2O3Whisker Ce-TZP complex phase mixed slurries are placed in beaker, and beaker is placed in into ultrasonic wave cleaning
In machine, while using blade type stirrer, supersonic synergic stirring 30min.
By the Al prepared by comparative example 1 of the present invention2O3Whiskers high-toughenedization Ce-TZP complex phase ceramic sections are scanned electronic display
Micro mirror is observed, as a result as shown in figure 3, Fig. 3 is the Al prepared by comparative example 1 of the present invention2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics
The scanning electron microscope (SEM) photograph of section, wherein, Al 1., 2., 3. prepared by comparative example 12O3Whiskers high-toughenedization Ce-TZP complex phase ceramics are brilliant
The reunion of palpus, microstructure defect.As shown in Figure 3：Al prepared by the method for comparative example 12O3Whiskers high-toughenedization Ce-TZP complex phases are made pottery
Porcelain is poor due to whisker dispersion effect, causes whisker agglomeration, microstructure uneven, so as to can not be densified.
Comparative example 2
Al is prepared according to the method for embodiment 12O3Whisker is combined Ce-TZP ceramic powders, as different from Example 1, step
Suddenly 2-amino-2-methyl-1-propanol (AMP-95) is replaced with into aluminium isopropoxide as whisker dispersant in (2).
By the Al prepared by comparative example 2 of the present invention2O3Whiskers high-toughenedization Ce-TZP complex phase ceramic sections are scanned electronic display
Micro mirror is observed, as a result as shown in figure 4, Fig. 4 is the Al prepared by comparative example 2 of the present invention2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics
The scanning electron microscope (SEM) photograph of section.As seen from Figure 4：Separated out using aluminium isopropoxide as whisker dispersant in sintering process
Al2O3, cause microstructure defect, so as to can not be densified.
As seen from the above embodiment, the invention provides a kind of high length-diameter ratio Al2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics
Preparation method, comprise the following steps：A) after mixing water, polyethylene glycol and 2-amino-2-methyl-1-propanol, pH value is adjusted
To 10~11, then and Al2O3Whisker is mixed, and under conditions of ultrasound and stirring, ball milling obtains the Al of different draw ratios2O3It is brilliant
Must slurry；B) under conditions of ultrasound and stirring, by the Al2O3Whisker slurry and the mixing of Ce-TZP powders, obtain complex phase mixing
Slurry；C) by the complex phase mixed slurry carry out ball milling, regulation pH value to 10~11, then successively carry out blade stirring, drying and
Sieving, obtains composite ceramic material；D) composite ceramic material is heated after dry-pressing, cold isostatic compaction, obtains green compact；
E) by the green sintering, high length-diameter ratio Al is obtained2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics.This method is with CeO2Stable Oxygen
Change zirconium (Ce-TZP) powder is raw material, Al2O3Whisker mends tough phase for enhancing, by Al2O3The scattered place of whisker and slurry
Reason, then be sintered, you can realize high length-diameter ratio Al2O3The complete densification of whiskers high-toughenedization Ce-TZP complex phase ceramics, has it
There is higher intensity and toughness.Test result indicates that：High length-diameter ratio Al2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics it is relatively close
Degree is higher than 99%, high length-diameter ratio Al2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics fracture toughness is 10~15MPam1/2, bending resistance
Intensity is 500~1000MPa.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of high length-diameter ratio alumina whisker Strengthening and Toughening Ce-TZP complex phase ceramic preparation methods, comprise the following steps：
A) will be after water, polyethylene glycol and 2-amino-2-methyl-1-propanol mix, then and Al regulation pH value is to 10~11,2O3It is brilliant
It must mix, under conditions of ultrasound and stirring, ball milling obtains the Al of different draw ratios2O3Whisker slurry；
B) under conditions of ultrasound and stirring, by the Al2O3Whisker slurry and the mixing of Ce-TZP powders, obtain complex phase mixing slurry
Material；
C) by the complex phase mixed slurry ball milling, regulation pH value is to 10~11, then progress blade stirring, dried and screened successively,
Obtain composite ceramic material；
D) composite ceramic material is heated after dry-pressing, cold isostatic compaction, obtains green compact；
E) by the green sintering, high length-diameter ratio Al is obtained2O3Whiskers high-toughenedization Ce-TZP complex phase ceramics.
2. preparation method according to claim 1, it is characterised in that Al in the step a)2O3The initial draw ratio of whisker
For 42~78.
3. preparation method according to claim 1, it is characterised in that Al in the step a)2O3Whisker accounts for the complex phase and mixed
Close 5~15vol% of solid powder content in slurry.
4. preparation method according to claim 1, it is characterised in that solid content in complex phase mixed slurry in the step b)
For 20~30vol%；Ce-TZP powders account for 85~95vol% of solid powder content in the complex phase mixed slurry.
5. preparation method according to claim 1, it is characterised in that complex phase mixed slurry ball milling turns in the step c)
Speed is 50~70rpm；The time of the complex phase mixed slurry ball milling is 10~20min.
6. preparation method according to claim 1, it is characterised in that in the step c) temperature of blade stirring be 55~
65℃；The time of blade stirring is 9~11h；The speed of blade stirring is 180~220rpm.
7. preparation method according to claim 1, it is characterised in that the temperature of heating is 550~650 in the step d)
℃；The time of heating is 1~2h.
8. preparation method according to claim 1, it is characterised in that in the step e) temperature of sintering for 1400~
1450℃；The time of sintering is 0.5~1h；The atmosphere of sintering is air atmosphere；The pressure of sintering is normal pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710471191.3A CN107056316B (en) | 2017-06-20 | 2017-06-20 | Preparation method of high-length-diameter-ratio alumina whisker toughened Ce-TZP multiphase ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710471191.3A CN107056316B (en) | 2017-06-20 | 2017-06-20 | Preparation method of high-length-diameter-ratio alumina whisker toughened Ce-TZP multiphase ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107056316A true CN107056316A (en) | 2017-08-18 |
| CN107056316B CN107056316B (en) | 2020-05-19 |
Family
ID=59594772
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710471191.3A Active CN107056316B (en) | 2017-06-20 | 2017-06-20 | Preparation method of high-length-diameter-ratio alumina whisker toughened Ce-TZP multiphase ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107056316B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456002A (en) * | 2018-02-08 | 2018-08-28 | 广东工业大学 | A method of being suitable for the 3D printing ceramic component based on Stereolithography of selfreparing/self-reinforcing |
| CN112592195A (en) * | 2020-12-02 | 2021-04-02 | 无锡市高宇晟新材料科技有限公司 | Complex phase microwave dielectric ceramic material and preparation method thereof |
| CN114351134A (en) * | 2021-11-23 | 2022-04-15 | 兆山科技（北京）有限公司 | Crack-resistant high-temperature-corrosion-resistant gradient ceramic coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104649698A (en) * | 2014-12-31 | 2015-05-27 | 东莞深圳清华大学研究院创新中心 | Method for dispersing monocrystalline sapphire fibers in zirconia ceramic composite material and composite material |
-
2017
- 2017-06-20 CN CN201710471191.3A patent/CN107056316B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104649698A (en) * | 2014-12-31 | 2015-05-27 | 东莞深圳清华大学研究院创新中心 | Method for dispersing monocrystalline sapphire fibers in zirconia ceramic composite material and composite material |
Non-Patent Citations (6)
| Title |
|---|
| 孙静: "稳定氧化锆陶瓷的研究现状", 《机械工程材料》 * |
| 朱和国: "《耐高温隔热材料技术》", 31 July 2013, 国防工业出版社 * |
| 朵英贤: "《纳米塑料技术》", 31 December 2006, 浙江科学技术出版社 * |
| 李见: "《新型材料导论》", 30 November 1987, 冶金工业出版社 * |
| 王成文: "SiC晶须的分散研究", 《苏州科技学院学报（工程技术版）》 * |
| 耿耀宗: "《现代水性涂料 工艺•配方•应用》", 31 March 2003, 中国石化出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456002A (en) * | 2018-02-08 | 2018-08-28 | 广东工业大学 | A method of being suitable for the 3D printing ceramic component based on Stereolithography of selfreparing/self-reinforcing |
| CN108456002B (en) * | 2018-02-08 | 2021-03-16 | 广东工业大学 | Method for 3D printing of ceramic component based on photocuring forming and suitable for self-repairing/self-enhancing |
| CN112592195A (en) * | 2020-12-02 | 2021-04-02 | 无锡市高宇晟新材料科技有限公司 | Complex phase microwave dielectric ceramic material and preparation method thereof |
| CN114351134A (en) * | 2021-11-23 | 2022-04-15 | 兆山科技（北京）有限公司 | Crack-resistant high-temperature-corrosion-resistant gradient ceramic coating and preparation method thereof |
| CN114351134B (en) * | 2021-11-23 | 2023-10-31 | 兆山科技（北京）有限公司 | Crack-resistant high-temperature corrosion-resistant gradient ceramic coating and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107056316B (en) | 2020-05-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107759218B (en) | Yttria-stabilized zirconia ceramic and preparation method thereof | |
| Vasylkiv et al. | Low‐temperature processing and mechanical properties of zirconia and zirconia–alumina nanoceramics | |
| Galassi et al. | Processing and characterization of high Qm ferroelectric ceramics | |
| Yu et al. | Fabrication of Nd: YAG transparent ceramics using powders synthesized by citrate sol-gel method | |
| CN107056316A (en) | A kind of preparation method of high length-diameter ratio alumina whisker Strengthening and Toughening Ce TZP complex phase ceramics | |
| CN109650885A (en) | One kind mixing lanthanum niobate silver lead-free anti-ferroelectric energy storage ceramic material and preparation method thereof | |
| JP4465173B2 (en) | Composite ceramics and manufacturing method thereof | |
| CN108530057B (en) | Preparation of morphology-controllable CaTiO applied to energy storage by sol-gel method3Method for producing ceramic | |
| CN101805178A (en) | High-energy ball milling preparation method of barium titanate-based semiconductor ceramics | |
| CN103613382A (en) | Sodium bismuth titanate-barium titanate-potassium bismuth titanate lead-free piezoelectric texture ceramic and preparation method thereof | |
| CN106495689B (en) | The preparation method of black zirconia ceramics | |
| CN108341668B (en) | Black zirconia ceramic and preparation method thereof | |
| CN112851342B (en) | Zirconia ceramic material and preparation method and application thereof | |
| CN106045505A (en) | Preparation method of magnesium oxide doped yttria-stabilized zirconia (5Y-PSZ) ceramic | |
| CN109608194A (en) | A kind of lead zirconate titanate thick film ceramics and its preparation method and application | |
| CN108727001B (en) | Zirconium dioxide toughened plate flaky alumina-based composite ceramic and preparation method thereof | |
| JP2019501855A (en) | Zr-based composite ceramic material, method for preparing the same, outer shell, or decorative material | |
| JP2004115343A (en) | Method of producing partially stabilized zirconia sintered compact | |
| CN109180185A (en) | A kind of method that ultra-short Time prepares high energy storage potassium-sodium niobate ferroelectric ceramic material | |
| CN109456055A (en) | A kind of high breakdown high polarization bismuth-sodium titanate ceramic material, preparation method and application | |
| CN101428850A (en) | Production method of barium titanate | |
| JP2004075425A (en) | Partially stabilized zirconia sintered compact | |
| CN105384436B (en) | A kind of barium-strontium titanate-based dielectric ceramic material of rich titanium-type and preparation method thereof | |
| CN1238304C (en) | Method for preparing Al4SiC4 ceramics | |
| CN105601283A (en) | Making method for Si3N4 ceramic of conductive network structure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |