CN108439978A - A kind of yttria-stabilized zirconia powder and preparation method thereof and ceramics - Google Patents
A kind of yttria-stabilized zirconia powder and preparation method thereof and ceramics Download PDFInfo
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- 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
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- 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
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention belongs to technical field of powdered material preparation, a kind of yttria-stabilized zirconia powder and preparation method thereof and ceramics are specifically provided.The present invention coats yttrium oxide powder using cationic surfactant, coats Zirconium powder using anion surfactant, then act on by electrostatic attraction, obtains the powder that yttrium oxide uniformly coats zirconium oxide.The ceramics being prepared using the present invention, relative density are 98.7~99.5%；Hardness reaches 1352~1432HV, and fracture toughness reaches 4.47~4.82MPam1/2。
Description
Technical field
The invention belongs to technical field of powdered material preparation more particularly to a kind of yttria-stabilized zirconia powder and its systems
Preparation Method and ceramics.
Background technology
Zirconium oxide has high intensity, high rigidity and good biocompatibility, can be used for making dentistry, human skeleton etc. raw
Object material, it can also be used to make the ceramic composite of fine structure.But after pure zirconia contacts vapor, easy aging is opened
It splits, therefore, the prior art usually adds yttrium oxide as stabilizer into zirconium oxide, prepares yttria-stabilized zirconia powder.
Currently, the method for industrially prepared yttria-stabilized zirconia powder has mechanical mixing and coprecipitation, wherein mechanical mixing
It is more common a kind of.Mechanical mixing is directly to mix yttrium oxide and Zirconium powder, makes yttrium oxide point by ball milling
Cloth is in zirconium surface, to obtain a kind of preparation method of yttria-stabilized zirconia powder.
Although mechanical mixing disclosed in the prior art can obtain yttria-stabilized zirconia powder, gained powder
Yttrium oxide can not be evenly coated at the surface of zirconium oxide, cause to occur secondary recrystallization in sintering process or part is coarse
Change, directly affect zirconia ceramic product at mutually and mechanical performance.
Invention content
The purpose of the present invention is to provide a kind of preparation method of yttria-stabilized zirconia powder, systems provided by the invention
Preparation Method can obtain the Zirconium powder of coated with uniform yttrium oxide layer, utilize gained yttria-stabilized zirconia powder system
Standby obtained ceramics have higher hardness and toughness.
In order to achieve the above object, the present invention provides a kind of preparation methods of yttria-stabilized zirconia powder, including such as
Lower step：
A kind of preparation method of yttria-stabilized zirconia powder, includes the following steps：
(1) yttrium oxide powder and cationic surfactant are distributed in deionized water, obtain yttrium oxide dispersion liquid；
The Zirconium powder and anion surfactant are distributed in deionized water, Zirconium oxide dispersion liquid is obtained；
The grain size of the yttrium oxide powder and Zirconium powder ratio is 1:5~20；
(2) under AC field and stirring condition, yttrium oxide dispersion liquid and zirconium oxide that the step (1) is obtained disperse
Liquid mixes, and is coated, and the slurry of yttrium oxide cladding zirconium oxide is obtained；The mass ratio of yttrium oxide and zirconium oxide is in the slurry
1:4~20；
(3) slurry that the step (2) obtains is dried and is crushed successively, obtain yttria-stabilized zirconia powder
Body.
Preferably, in the step (1), the mass ratio of yttrium oxide powder and cationic surfactant is 1:0.003~
0.005, the solid content of the yttrium oxide dispersion liquid is 20~30%, and the solid content accounts for yttrium oxide dispersion liquid total amount with yttrium oxide
Mass percent meter；
The mass ratio of Zirconium powder and anion surfactant is 1:0.003~0.005, the Zirconium oxide dispersion liquid
Solid content be 20~30%, the solid content is in terms of the mass percent that zirconium oxide accounts for Zirconium oxide dispersion liquid total amount.
Preferably, the grain size of yttrium oxide powder is 40~60nm in the step (1).
Preferably, cationic surfactant includes halogenated phosphates or cetyl three in the step (1)
Methyl bromide ammonium；The anion surfactant includes NaTDC or polymethylacrylic acid.
Preferably, the preparation method of yttrium oxide dispersion liquid includes in the step (1)：
Cationic surfactant is dissolved in portions of de-ionized water, it is water-soluble to obtain cationic surfactant deionization
Liquid；
After the cationic surfactant deionized water solution is mixed with yttrium oxide powder and remaining deionized water,
Ball milling obtains yttrium oxide dispersion liquid.
Preferably, the preparation method of Zirconium oxide dispersion liquid includes in the step (1)：By the Zirconium powder, it is cloudy from
Ball milling after sub- surfactant is mixed with deionized water, obtains Zirconium oxide dispersion liquid.
Preferably, the hybrid mode of yttrium oxide dispersion liquid and Zirconium oxide dispersion liquid is to be added dropwise in the step (2), the drop
The speed added is 0.8~2mL/s.
Preferably, the frequency of AC field is 45~55Hz in the step (2)；The power-on voltage of the AC field is
The conduction time of 2~8V, the AC field are 2~5h.
The present invention also provides the yttria-stabilized zirconia powder that preparation method described in above-mentioned technical proposal is prepared,
There is the yttria-stabilized zirconia powder nucleocapsid, the nucleocapsid to include zirconium oxide nucleome and pass through electrostatic interaction
The yttrium oxide shell of absorption；The zirconium oxide core surface is negatively charged, and the yttrium oxide shell is by the positively charged oxygen in surface
Change yttrium particle composition；
The thickness of yttrium oxide shell is 60~150nm in the yttria-stabilized zirconia powder.
The present invention also provides a kind of ceramics, yttria-stabilized zirconia powder described in the ceramics techniques described above scheme
For raw material, repressed and sintering obtains.
The present invention provides a kind of preparation methods of yttria-stabilized zirconia powder, include the following steps：By yttrium oxide
Powder and cationic surfactant are distributed in deionized water, obtain yttrium oxide dispersion liquid；By the Zirconium powder and the moon
Ionic surface active agent is distributed in deionized water, obtains Zirconium oxide dispersion liquid；The yttrium oxide powder and Zirconium powder
Grain size ratio is 1:5~20；Under AC field and stirring condition, obtained yttrium oxide dispersion liquid and Zirconium oxide dispersion liquid are mixed
It closes, is coated, obtain the slurry of yttrium oxide cladding zirconium oxide；The mass ratio of yttrium oxide and zirconium oxide is 1 in the slurry:4
~20；Obtained slurry is dried and is crushed successively, yttria-stabilized zirconia powder is obtained.
The present invention mixes cationic surfactant with yttrium oxide powder, by anion surfactant and zirconia powder
Body mixes, and the surface of yttrium oxide powder and Zirconium powder can be made to be respectively coated by cationic surfactant and anionic surface work
Property agent, and then obtain the negatively charged zirconia particles of the positively charged yttria particles in surface and surface；In AC field and
Under stirring condition, the positively charged yttria particles in the surface zirconia particles negatively charged with surface constantly move, and are moved through
Cheng Zhong, positive charge and negative electrical charge are acted on by coulomb electrostatic attraction, and yttria particles and zirconia particles is promoted to attract each other；And
And yttria particles grain size is small, and zirconia particles grain size is big, when two kinds of particles are close to each other, including zirconia particles, and yttrium oxide
Particle forms the nucleocapsid of yttrium oxide cladding zirconium oxide in outer layer；Further, since yttria particles surface carries positive charge,
Like charges are mutually exclusive, promote yttria particles that can uniformly be arranged in the surface of zirconia particles, form uniform oxidation
Yttrium clad.Using the yttria-stabilized zirconia powder that is prepared of the present invention, can obtain into mutually uniformly, and mechanical performance compared with
Good ceramic.
Embodiment the result shows that, the clad uniformity of yttria-stabilized zirconia powder obtained by the application is preferable, sintering
The relative density of gained ceramics is 98.7~99.5% afterwards；Hardness reaches 1352~1432HV, and fracture toughness reaches 4.47~
4.82MPa·m1/2。
Description of the drawings
Fig. 1 is the effect contrast figure that mechanical mixing and the method for the present invention prepare yttria-stabilized zirconia powder；
Fig. 2 is the mechanism schematic diagram that the present invention prepares yttria-stabilized zirconia powder；
Fig. 3 is that the SEM of 1 gained yttria-stabilized zirconia powder of embodiment schemes；
Fig. 4 is that the SEM of 1 gained yttria-stabilized zirconia powder of comparative example schemes；
Fig. 5 is that the TEM of 1 gained yttria-stabilized zirconia powder of embodiment schemes.
Specific implementation mode
The present invention provides a kind of preparation methods of yttria-stabilized zirconia powder, include the following steps：
(1) yttrium oxide powder and cationic surfactant are distributed in deionized water, obtain yttrium oxide dispersion liquid；
The Zirconium powder and anion surfactant are distributed in deionized water, Zirconium oxide dispersion liquid is obtained；
The grain size of the yttrium oxide powder and Zirconium powder ratio is 1:5~20；
(2) under AC field and stirring condition, yttrium oxide dispersion liquid and zirconium oxide that the step (1) is obtained disperse
Liquid mixes, and is coated, and the slurry of yttrium oxide cladding zirconium oxide is obtained；The mass ratio of yttrium oxide and zirconium oxide is in the slurry
1:4~20；
(3) slurry that the step (2) obtains is dried and is crushed successively, obtain yttria-stabilized zirconia powder
Body.
In the present invention, raw material and reagent are used in the preparation method of the yttria-stabilized zirconia powder, except special
It is commercial product well known to those skilled in the art outside illustrating.
Yttrium oxide powder and cationic surfactant are distributed in deionized water by the present invention, obtain yttrium oxide dispersion
Liquid.In the present invention, the grain size of the yttrium oxide powder is preferably 40~60nm, further preferably 45~55nm.In this hair
In bright, the cationic surfactant preferably includes halogenated phosphates or cetyl trimethylammonium bromide
(CTAB), further preferably cetyl trimethylammonium bromide.
In the present invention, the mass ratio of the yttrium oxide powder and cationic surfactant is preferably 1:0.003~
0.005, further preferably 1:0.004.In the present invention, solid content accounts for the quality percentage of dispersion liquid total amount with yttrium oxide powder
Than meter, the solid content of the yttrium oxide dispersion liquid is preferably 20~30%, and further preferably 22~28%.
In the present invention, the preparation method of the yttrium oxide dispersion liquid preferably includes：
Cationic surfactant is dissolved in portions of de-ionized water, it is water-soluble to obtain cationic surfactant deionization
Liquid；
Obtained cationic surfactant deionized water solution, yttrium oxide powder and remaining deionized water are mixed
Afterwards, ball milling obtains yttrium oxide dispersion liquid.
The present invention does not have particular/special requirement to the specific implementation mode of the dissolving, is using well known to those skilled in the art
It can.In the present invention, when the cationic surfactant is CTAB, preferably 40~60 DEG C of the temperature of the dissolving, further
Preferably 45~55 DEG C, to accelerate the solution rate of CTAB.
The present invention does not have particular/special requirement to the concentration of the cationic surfactant deionized water solution, can realize sun
Ionic surface active agent fully dissolves.In the present invention, the cationic surfactant and dissolving deionized water
Mass ratio is preferably 1:8~20, further preferably 1:10~15.In the present invention, the cationic surfactant dissolving
Come from the raw material deionized water of the yttrium oxide dispersion liquid with deionized water.
After obtaining cationic surfactant deionized water solution, the present invention is by the cationic surfactant deionization
After aqueous solution, yttrium oxide powder and the mixing of remaining deionized water, ball milling obtains yttrium oxide dispersion liquid.The present invention is to the surface
The hybrid mode of activating agent deionized water solution, yttrium oxide powder and deionized water does not have particular/special requirement, using art technology
Hybrid mode known to personnel.After mixing, the present invention carries out ball milling to the mixed material, so that yttrium oxide powder
It can uniformly be mixed with cationic surfactant, and then form the positively charged yttria particles in surface.In the present invention, institute
The rotating speed for stating ball milling is preferably 400~800r/min, further preferably 450~700r/min；The time of the ball milling is preferred
For 1~6h, further preferably 2~5h.
The Zirconium powder and anion surfactant are distributed in deionized water by the present invention, obtain zirconium oxide point
Dispersion liquid.In the present invention, the grain size of the yttrium oxide powder and Zirconium powder is than preferably 1:5~20, further preferably
1:6~15.The grain size of the yttrium oxide powder and Zirconium powder is limited to above range by the present invention, can make the oxygen of small particle
Change the surface that yttrium is coated on big grain size zirconium oxide as clad material.In the present invention, the anion surfactant is excellent
Choosing includes NaTDC or polymethylacrylic acid, further preferably NaTDC.
In the present invention, the mass ratio of the Zirconium powder and anion surfactant is preferably 1:0.003~
0.005, further preferably 1:0.004.In the present invention, solid content accounts for the matter of Zirconium oxide dispersion liquid total amount with Zirconium powder
Percentages are measured, the solid content of the Zirconium oxide dispersion liquid is preferably 40-50%, and further preferably 42~48%.
In the present invention, the preparation method of the Zirconium oxide dispersion liquid preferably includes：By the Zirconium powder, anion
Ball milling after surfactant and deionized water mixing, obtains Zirconium oxide dispersion liquid.The present invention is to the Zirconium powder, anion
The hybrid mode of surfactant and deionized water does not have particular/special requirement, using mode well known to those skilled in the art.
After mixing, the present invention preferably carries out ball milling to the mixed material, so that Zirconium powder and anion surfactant
It can uniformly mix, and then obtain the negatively charged zirconia particles in surface.In the present invention, the rotating speed of the ball milling is preferably
400~800r/min, further preferably 450~750r/min；The time of the ball milling is preferably 1~6h, further preferably
For 2~5h.
When ball milling, in mass, the ratio of grinding media to material of the ball milling is preferably 1~3:1, further preferably 2:1；The ball milling
It is preferably 4~9mm with the diameter of abrading-ball, further preferably 5~8mm；The material of the ball milling is preferably zirconia ball.This hair
The bright specific implementation mode to the ball milling does not have particular/special requirement, using well known to those skilled in the art.
In the present invention, point of the preparation sequence without time order and function of the yttrium oxide dispersion liquid and Zirconium oxide dispersion liquid.
After obtaining yttrium oxide dispersion liquid and Zirconium oxide dispersion liquid, under AC field and stirring condition, the present invention will be described
Yttrium oxide dispersion liquid and Zirconium oxide dispersion liquid mixing, are coated, and the slurry of yttrium oxide cladding zirconium oxide is obtained.In the present invention
In, yttrium oxide and zirconium oxide mass ratio in the Zirconium oxide dispersion liquid are 1 in the yttrium oxide dispersion liquid:3~20, it is further excellent
It is selected as 1:4~18, more preferably 1:5~15.In the present invention, the mode of the mixing is preferably added dropwise, the speed of the dropwise addition
Degree is preferably 0.8~2mL/s, further preferably 1.0~1.8mL/s, more preferably 1.2~1.6mL/s.In the present invention,
The dropwise addition can add to the yttrium oxide dispersant liquid drop in Zirconium oxide dispersion liquid, can also be to disperse the zirconium oxide
Drop adds in the yttrium oxide dispersion liquid.The present invention mixed oxidization yttrium dispersion liquid and zirconium oxide dispersion by the way of being added dropwise
Liquid can provide the sufficient time for the cladding of yttrium oxide and zirconium oxide, and avoiding addition excessively influences the uniformity of clad.
In the present invention, the mixing of the yttrium oxide dispersion liquid and Zirconium oxide dispersion liquid, be coated on AC field and stirring
Under the conditions of carry out.In the present invention, the frequency of the AC field is preferably 45~55Hz, further preferably 48~52Hz；
The power-on voltage of the AC field is preferably 2~8V, further preferably 3~7V；The conduction time of the AC field is excellent
It is selected as 2~5h, further preferably 3~4h.Preferably the AC field of capsulation condition is arranged in above-mentioned condition, to carry by the present invention
High covered effect obtains the uniform yttria-stabilized zirconia powder of clad.The present invention carries the specific of the AC field
There is no particular/special requirement for mode, using mode well known to those skilled in the art.
In the present invention, the speed of the stirring is preferably 500~700r/min, further preferably 550~650r/
min；The mixing time is preferably 2~5h, further preferably 2.5~4h.
The present invention, by the mixing of the yttrium oxide dispersion liquid and Zirconium oxide dispersion liquid, makes under AC field and stirring condition
The zirconia particles that yttria particles and surface of the surface with positive charge carry negative electrical charge constantly move, in motion process just,
Negative electrical charge attracts each other to form yttria-stabilized zirconia powder by the effect of coulomb electrostatic attraction.
For clear interpretation covered effect of the present invention, by the design sketch of the cladding process of the present invention and products obtained therefrom and routine
Mechanical mixing carries out comparative illustration.As shown in Figure 1, A indicates that mechanical mixing, B indicate the preparation method of the present invention, wherein Z
Indicate that zirconium oxide, Y indicate yttrium oxide；As shown in Figure 1, under conditions of using same materials, oxygen is prepared using mechanical mixing
When changing yttrium stable zirconium oxide powder, yttrium oxide mixes uneven with zirconium oxide, and yttrium oxide is not formed on the surface of zirconium oxide
Even clad structure；And the preparation method of the present invention is utilized, yttrium oxide can be evenly coated at the surface of zirconium oxide.
The present invention realizes that yttrium oxide uniformly coats the mechanism of Zirconium powder as shown in Fig. 2, Z indicates zirconium oxide, Y tables in figure
Show yttrium oxide, m indicates anion surfactant, and n indicates cationic surfactant, I indicate zirconium surface cladding it is cloudy from
The process of sub- surfactant, II indicate that the process of yttria surfaces cladding cationic surfactant, III indicate that yttrium oxide is steady
Determine the forming process of Zirconium powder.
As shown in Fig. 2, after the present invention mixes anion surfactant m with Zirconium powder Z, anion surface active
Agent m is coated on the surface of Zirconium powder Z, forms the negatively charged zirconia particles in surface；Cationic surfactant n and oxygen
After changing the Y mixing of yttrium powder body, cationic surfactant n is coated on the surface of yttrium oxide powder Y, forms the negatively charged oxygen in surface
Change yttrium particle；After the negatively charged zirconia particles in the surface yttria particles positively charged with surface mix, positive charge with it is negative
Charge attracts each other, and the grain size of zirconia particles is larger, and the grain size of yttria particles is smaller, therefore, forms yttrium oxide cladding
The nucleocapsid of zirconium oxide；In addition, since yttria surfaces carry positive charge, then due to electricity of the same race between yttrium oxide and yttrium oxide
Lotus is mutually exclusive, so that the yttria particles with positive charge is evenly distributed on the surface of zirconium oxide, avoids accumulating, and then wrapped
The more uniform yttria-stabilized zirconia powder of coating.
After obtaining slurry, the present invention is dried and crushes successively to the slurry, obtains yttria-stabilized zirconia powder
Body.In the present invention, the temperature of the drying is preferably 40~100 DEG C, further preferably 45~90 DEG C；The drying when
Between preferably 5~25h, further preferably 6~20h.The present invention does not have particular/special requirement to the specific implementation mode of the drying,
Using mode well known to those skilled in the art.
After the drying, the present invention crushes the material after drying, obtains yttria-stabilized zirconia powder.At this
In invention, the material after the drying is bulk, is crushed to it, can obtain yttria-stabilized zirconia powder.The present invention
There is no particular/special requirement to the specific implementation mode of the crushing, using mode well known to those skilled in the art.
After the crushing, the present invention is preferably sieved to crushing rear material, is aoxidized using screenings as stabilized with yttrium oxide
Zirconium powder body.In the present invention, the sieving is preferably 80~200 mesh with sieve, further preferably 100~150 mesh.The present invention
There is no particular/special requirement to the specific implementation mode of the sieving, using mode well known to those skilled in the art.
The present invention provides yttria-stabilized zirconia powder described in above-mentioned technical proposal, the yttria-stabilized zirconia
It includes zirconium oxide nucleome and the yttrium oxide shell that is adsorbed by electrostatic interaction that powder, which has nucleocapsid, the nucleocapsid,；Institute
State that zirconium oxide core surface is negatively charged, the yttrium oxide shell is made of the positively charged yttrium oxide powder in surface.In this hair
In bright, the cationic surfactant of the yttrium oxide cladding and the anion surfactant of zirconium surface cladding are less,
Quality is negligible, the mass ratio of the yttrium oxide shell and zirconium oxide nucleome preferably with yttrium oxide raw material and zirconia material
Mass ratio it is consistent, be not repeated herein.In the present invention, in the yttria-stabilized zirconia powder yttrium oxide shell thickness
Degree is 60~150nm, further preferably 80~120nm.
In the present invention, the anion surfactant in the yttria-stabilized zirconia powder and cationic surface are lived
Property agent dosage it is less, be used as ceramic raw material when, can prepare ceramics during by be sintered remove, yttrium oxide can't be influenced
The sintering character and mechanical performance of stable peroxide zirconium powder body.
The present invention also provides a kind of ceramics, yttria-stabilized zirconia powder described in the ceramics techniques described above scheme
For raw material, repressed and sintering obtains.
The present invention first suppresses the yttria-stabilized zirconia powder, to obtain suitable for sintering into parison.
In the present invention, the compacting is preferably isostatic pressed, further preferably isostatic cool pressing.In the present invention, the pressure of the isostatic pressed
It is preferably 200~240MPa, further preferably 205~220MPa by force；The dwell time of the isostatic pressed is preferably 8~
12min, further preferably 9~10min；Isostatic pressed of the present invention preferably carries out at ambient temperature.The present invention is to described
The specific implementation mode of isostatic pressed does not have particular/special requirement, using well known to those skilled in the art.
After compacting, the present invention is sintered to what is obtained after the compacting at parison, obtains ceramics.In the present invention, institute
The temperature for stating sintering is preferably 1440~1480 DEG C, further preferably 1445~1460 DEG C；The time of the heat preservation is preferably
2.8~4h, further preferably 3~3.5h.After sintering, the present invention preferably cools down the sintered blank base obtained after sintering,
Obtain ceramics.The present invention does not have particular/special requirement to the mode of the cooling, using well known to those skilled in the art.At this
In inventive embodiments, the cooling is preferably natural cooling.
Ceramics of the present invention have uniform phase constitution and excellent mechanical performance.In the present invention, it is described ceramics
Hardness preferably >=1350HV, further preferably 1352~1432HV；The toughness of the ceramics is preferably >=4.45MPam1/2,
Further preferably 4.46~4.82MPam1/2。
In order to further illustrate the present invention, stabilized with yttrium oxide provided by the invention is aoxidized with reference to the accompanying drawings and examples
Zirconium and preparation method thereof and ceramics are described in detail, but cannot they be interpreted as limiting the scope of the present invention.
Embodiment 1
Zirconium powder grain size is 300nm, and yttrium oxide powder grain size is 50nm；800 parts of Zirconium powders, 3.2 parts are taken off
Oxycholic acid sodium and 1000 parts of deionized water mixing, obtain Zirconium oxide dispersion liquid；By 200 parts of yttrium oxide powders, 0.8 part of cetyl
Trimethylammonium bromide and 300 parts of deionized water mixing, obtain yttrium oxide dispersion liquid；
Zirconium oxide dispersion liquid is fitted into glass container, then apply voltage be 8V, the AC field that frequency is 50Hz, stir
Under the conditions of mixing, yttrium oxide dispersion liquid is added dropwise, rate of addition 1mL/s after being added dropwise, continues to stir 3h, obtains mixture；
Mixture is placed in drying box, it is dry at 40 DEG C to obtain dry blocky powder for 24 hours, 80 mesh are crossed after grinding
Sieve, screenings is yttria-stabilized zirconia powder.
Gained stabilized with yttrium oxide peroxidating zirconium powder body is sintered under the following conditions：Pressurize 9min, obtains at 230MPa
At parison, then 4.5h will be kept the temperature at parison at 1475 DEG C, and after cooled to room temperature, obtain ceramics.
Embodiment 2
Zirconium powder grain size is 500nm, and yttrium oxide powder grain size is 50nm；850 parts of Zirconium powders, 3.4 parts are gathered
Methacrylic acid and 1200 parts of deionized water mixing, then ball milling 3h under conditions of 480r/min, obtains Zirconium oxide dispersion liquid；
It takes 0.6 part of cetyl trimethylammonium bromide to be added in 10mL deionization deionized waters, be heated to 50 DEG C and stir
It mixes, stops stirring and heating after solution clarification, obtain cetyl trimethylammonium bromide deionized water solution；150 parts are aoxidized
Yttrium powder body is added in cetyl trimethylammonium bromide deionized water solution, and ball milling 3h, obtains under conditions of 480r/min
Yttrium oxide dispersion liquid；
Yttrium oxide dispersion liquid is fitted into glass container, then apply voltage be 6V, the AC field that frequency is 48Hz, stir
Under the conditions of mixing, Zirconium oxide dispersion liquid is added dropwise, rate of addition 1.2mL/s after being added dropwise, continues to stir 4h, obtains mixture；
Mixture is placed in drying box, dry 18h, obtains dry blocky powder at 60 DEG C, and 150 mesh are crossed after grinding
Sieve, screenings is yttria-stabilized zirconia powder.
It is sintered yttria-stabilized zirconia powder obtained by the present embodiment according to the method for embodiment 1, obtains ceramics, difference
It is 208MPa to be in pressure when compression moulding, and dwell time 8min, sintering temperature is 1500 DEG C, soaking time 4h.
Embodiment 3
Zirconium powder grain size is 300nm, and yttrium oxide powder grain size is 40nm；900 parts of Zirconium powders, 2.7 parts are taken off
Oxycholic acid sodium and 1200 parts of deionized water mixing, then ball milling 4h under conditions of 400r/min, obtains Zirconium oxide dispersion liquid；
100 parts of yttrium oxide powders, 0.3 part of halogenated phosphates and 200 parts of deionized waters are mixed, in 480r/min
Under conditions of ball milling 3h, obtain yttrium oxide dispersion liquid；
Zirconium oxide dispersion liquid is fitted into glass container, then apply voltage be 4V, the AC field that frequency is 52Hz, stir
Under the conditions of mixing, yttrium oxide dispersion liquid is added dropwise, rate of addition 1.2mL/s after being added dropwise, continues to stir 3h, obtains mixture；
Mixture is placed in drying box, dry 12h, obtains dry blocky powder at 80 DEG C, and 120 mesh are crossed after grinding
Sieve, screenings is yttria-stabilized zirconia powder.
It is sintered yttria-stabilized zirconia powder obtained by the present embodiment according to the method for embodiment 1, obtains ceramic, no
It is that pressure when compression moulding is 225MPa with place, dwell time 11min, sintering temperature is 1450 DEG C, soaking time
For 3h.
Embodiment 4
Zirconium powder grain size is 500nm, and yttrium oxide powder grain size is 60nm；950 parts of Zirconium powders, 4.75 parts are gathered
Sodium methacrylate and 1500 parts of deionized water mixing, then ball milling 3h under conditions of 480r/min, obtains zirconium oxide dispersion
Liquid；
It is 1 to take 0.15 part of cetyl trimethylammonium bromide mass ratio:1 is added in 8mL deionization deionized waters, heating
It to 50 DEG C and stirs, stops stirring and heating after solution clarification, obtain cetyl trimethylammonium bromide deionized water solution；It will
50 parts of yttrium oxide powders are added to cetyl trimethylammonium bromide deionized water solution, ball milling under conditions of 480r/min
3h obtains yttrium oxide dispersion liquid；
Yttrium oxide dispersion liquid is fitted into glass container, then apply voltage be 2V, the AC field that frequency is 50Hz, stir
Under the conditions of mixing, Zirconium oxide dispersion liquid is added dropwise, rate of addition 1.5mL/s after being added dropwise, continues to stir 3h, obtains mixture；
Mixture is placed in drying box, dry 6h, obtains dry blocky powder at 100 DEG C, and 100 mesh are crossed after grinding
Sieve, screenings is yttria-stabilized zirconia powder.
It is sintered yttria-stabilized zirconia powder obtained by the present embodiment according to the method for embodiment 1, obtains ceramic, no
It is that pressure when compression moulding is 200MPa with place, dwell time 10min, sintering temperature is 1485 DEG C, soaking time
For 3.5h.
Comparative example 1
Raw material is taken according to the scheme of embodiment 1, yttria-stabilized zirconia powder, ball are prepared using solid phase mechanical mixing
The rotating speed of mill is 480r/min, Ball-milling Time 12h, ratio of grinding media to material 1.5:1.It is steady according to the method test yttrium oxide of embodiment 1
Determine the performance parameter of Zirconium powder, the results are shown in Table 1.Ceramics, the performance of gained ceramics are prepared according to the condition of embodiment 4
It is listed in Table 1 below.
Using scanning electron microscope to the pattern of 1 gained yttria-stabilized zirconia powder of embodiment 1 and comparative example into
Row characterization, is shown in shown in Fig. 3 and Fig. 4.From the figure 3, it may be seen that the present invention prepares gained stabilized with yttrium oxide peroxidating zirconium powder body uniform particle sizes,
And the yttria-stabilized zirconia powder that comparative example 1 (Fig. 4) is prepared is reunited seriously, particle size is uneven, is not formed
Even clad influences the sintering character of powder, and then influences the phase structure and mechanical property of ceramic material.
Using the clad of yttria-stabilized zirconia powder obtained by transmission electron microscope characterization embodiment, as shown in Figure 5.By scheming
It is found that it is that yttrium oxide coats zirconium oxide composite granule, and yttrium oxide clad (light color portion in figure that the present invention, which prepares gained powder,
Point) thickness it is uniform.
Utilize the grain size of 1 yttria-stabilized zirconia powder of laser particle analyzer testing example 1~4 and comparative example, test
It the results are shown in Table 1.Particle size range indicates the minimum grain size and maximum particle diameter of gained yttria-stabilized zirconia powder in table 1, by counting
According to it is found that the particle size distribution range for the yttria-stabilized zirconia powder that the present invention is prepared is narrow, illustrate the homogeneity of powder
Preferably.And the particle size distribution range of 1 gained sample of comparative example is wider, homogeneity is poor.
Using indentation method, under 20kg active forces, pressurize 15s, 1 ceramics sample of testing example 1~4 and comparative example it is hard
Degree performance and toughness, test result are shown in Table 1.
1 Examples 1 to 4 of table and 1 yttria-stabilized zirconia powder of comparative example and ceramic performance
As shown in Table 1, the ceramics sample being prepared using yttria-stabilized zirconia powder obtained by the present invention relative to
For comparative example 1, hardness and toughness, which have, to be obviously improved, and illustrates that yttria-stabilized zirconia powder provided by the invention overcomes
Diameter of particle homogeneity poor problem, improves the sintering character of powder.
In conclusion the clad that preparation method provided by the invention can obtain yttria-stabilized zirconia powder is equal
It is even, and diameter of particle reaches Nano grade, it is advantageous to the sintering character for improving powder.With stabilized with yttrium oxide oxidation obtained by the present invention
Zirconium powder body is raw material, and the ceramics obtained after sintering have preferable hardness, fracture toughness and relative density, illustrate offer of the present invention
Yttria-stabilized zirconia as ceramic raw material in use, the ceramic of better mechanical property can be obtained.
In addition, method provided by the invention is simple and easy to control, manufacturing cost is relatively low, is suitable for large-scale promotion and uses.
Although above-described embodiment is made that detailed description to the present invention, it is only a part of the embodiment of the present invention,
Rather than whole embodiments, people can also obtain other embodiment according to the present embodiment under the premise of without creativeness, these
Embodiment belongs to the scope of the present invention.
Claims (10)
1. a kind of preparation method of yttria-stabilized zirconia powder, includes the following steps：
(1) yttrium oxide powder and cationic surfactant are distributed in deionized water, obtain yttrium oxide dispersion liquid；
The Zirconium powder and anion surfactant are distributed in deionized water, Zirconium oxide dispersion liquid is obtained；
The grain size of the yttrium oxide powder and Zirconium powder ratio is 1:5~20；
(2) under AC field and stirring condition, the yttrium oxide dispersion liquid and Zirconium oxide dispersion liquid that the step (1) is obtained are mixed
It closes, is coated, obtain the slurry of yttrium oxide cladding zirconium oxide；The mass ratio of yttrium oxide and zirconium oxide is 1 in the slurry:4
~20；
(3) slurry that the step (2) obtains is dried and is crushed successively, obtain yttria-stabilized zirconia powder.
2. preparation method as described in claim 1, which is characterized in that in the step (1), yttrium oxide powder and cation form
The mass ratio of face activating agent is 1:0.003~0.005, the solid content of the yttrium oxide dispersion liquid is 20~30%, described to contain admittedly
Amount is in terms of the mass percent that yttrium oxide accounts for yttrium oxide dispersion liquid total amount；
The mass ratio of Zirconium powder and anion surfactant is 1:0.003~0.005, the Zirconium oxide dispersion liquid is consolidated
Content is 20~30%, and the solid content is in terms of the mass percent that zirconium oxide accounts for Zirconium oxide dispersion liquid total amount.
3. preparation method as claimed in claim 1 or 2, which is characterized in that the grain size of yttrium oxide powder is in the step (1)
40~60nm.
4. preparation method as claimed in claim 1 or 2, which is characterized in that cationic surfactant packet in the step (1)
Include halogenated phosphates or cetyl trimethylammonium bromide；The anion surfactant include NaTDC or
Polymethylacrylic acid.
5. preparation method as claimed in claim 1 or 2, which is characterized in that the preparation of yttrium oxide dispersion liquid in the step (1)
Method includes：
Cationic surfactant is dissolved in portions of de-ionized water, cationic surfactant deionized water solution is obtained；
After the cationic surfactant deionized water solution is mixed with yttrium oxide powder and remaining deionized water, ball milling
Obtain yttrium oxide dispersion liquid.
6. preparation method as claimed in claim 1 or 2, which is characterized in that the preparation of Zirconium oxide dispersion liquid in the step (1)
Method includes：Ball milling after the Zirconium powder, anion surfactant are mixed with deionized water obtains zirconium oxide dispersion
Liquid.
7. preparation method as described in claim 1, which is characterized in that yttrium oxide dispersion liquid and zirconium oxide in the step (2)
The hybrid mode of dispersion liquid is to be added dropwise, and the speed of the dropwise addition is 0.8~2mL/s.
8. preparation method as claimed in claim 1 or 7, which is characterized in that the frequency of AC field is 45 in the step (2)
~55Hz；The power-on voltage of the AC field is 2~8V, and the conduction time of the AC field is 2~5h.
9. the yttria-stabilized zirconia powder that any one of claim 1~8 preparation method is prepared, the yttrium oxide
It includes zirconium oxide nucleome and the oxidation adsorbed by electrostatic interaction that oxide-stabilizing zirconia powder, which has nucleocapsid, the nucleocapsid,
Yttrium shell；The zirconium oxide core surface is negatively charged, and the yttrium oxide shell is by the positively charged yttria particles group in surface
At；
The thickness of yttrium oxide shell is 60~150nm in the yttria-stabilized zirconia powder.
10. a kind of ceramics, the ceramics are using yttria-stabilized zirconia powder described in claim 9 as raw material, repressed and burning
Knot obtains.
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