CN106938931A - High purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof - Google Patents

High purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof Download PDF

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CN106938931A
CN106938931A CN201710144563.1A CN201710144563A CN106938931A CN 106938931 A CN106938931 A CN 106938931A CN 201710144563 A CN201710144563 A CN 201710144563A CN 106938931 A CN106938931 A CN 106938931A
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zirconium oxide
stable zirconium
yttrium stable
oxide ceramics
preparation
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不公告发明人
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Nanjing Jinli New Material Co., Ltd
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Nanjing Cloud Qijin Rui New Material Co Ltd
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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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Abstract

The invention provides a kind of brand-new high purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof, granulated using high-purity Nano-class yttrium stable zirconium oxide powder by the method for centrifugal spray granulation, it is compressing by isostatic cool pressing, it is made finally by the method for HIP sintering, the present invention has the advantages that high purity high dense, not only technique and equipment are simple by the present invention, low cost, high income, energy consumption is low, production efficiency is high, it is adapted to industrialized production, and result in steady quality, the tiny controllable yttrium stable zirconium oxide ceramics of crystal grain, process of the present invention is without Environment pollution, it is a kind of new low cost, the preparation method of the high purity high dense yttrium stable zirconium oxide ceramics of steady quality.

Description

High purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof
Technical field
The invention belongs to technical field of material, and in particular to a kind of high purity high dense yttrium stable zirconium oxide ceramics and its Preparation method.
Background technology
Zirconium oxide is that it has the different phase of 3 kinds of structures, i.e. monoclinic phase, four using relatively extensive a kind of in ceramic material Side's phase and Emission in Cubic, different phase contents can produce large effect to the performance of zirconia ceramics material.At present, it is common The zirconia material that mostly yttrium is stablized.Wherein with 3Y-TZP（Teragonal zirconia polycrystals Stabilized, 3 molar fraction Y2O3）The mechanical property of material is optimal, and it is also a class zirconia ceramics the most frequently used at present Material, has broad application prospects in different industries, such as chemical industry, machinery.
Chinese patent 201110450949.8 provides a kind of flexible yttrium stable zirconium oxide ceramic fiber and preparation method thereof. The zirconia particles particle diameter for constituting ceramic fibre is 10-400nm, and a diameter of 0.5-3 μm of ceramic fibre, fiber is uniform and continuous, It is not easy to break, there is good pliability.Combined using sol-gel process with electrostatic spinning technique and prepared zirconium oxide gelatinous fibre, Yttrium stable zirconium oxide ceramic fiber is obtained after gelatinous fibre is calcined.The heat endurance of gained yttrium stable zirconium oxide ceramic fiber Good, mechanical property is excellent, can also act as battery diaphragm and high temperature mistake as high temperature catalyst support and high temperature insulating material Filter etc..
Chinese patent 201310125398.7 provides a kind of tetragonal phase zirconium oxide ceramics 3Y- of tooth stabilized with yttrium oxide TZP preparation method, processing step is：（1）3Y-TZP suspension and aluminum saline solution are prepared respectively, by the aluminum saline solution It is added drop-wise in the 3Y-TZP suspension, is formed in well mixed 3Y-TZP powders-aluminium salt mixed liquor, the mixed liquor, Al3+ Concentration control is in 0.01mol/L ~ 0.23mol/L, content control 10wt%~20wt% of 3Y-TZP powders；（2）In step（1）System Urea is added in standby 3Y-TZP powders-aluminium salt mixed liquor, and 2h~3h is incubated at 70 DEG C~85 DEG C, aluminium hydroxide cladding is obtained 3Y-TZP powders slurry, remove impurity with pure water washing by the slurries filtration, and by filtering gained solid matter, it is dry Dry and calcining, crushes, that is, obtains Surface coating Al2O33Y-TZP powders；（3）By Surface coating Al2O33Y-TZP powders into Type and sintering, obtain the tetragonal phase zirconium oxide ceramics 3Y-TZP of tooth stabilized with yttrium oxide.
Chinese patent 200410025548.8 provides a kind of neodymia and yttrium oxide co-stabilized tetragonal zirconia polycrystal （Nd, Y）- TZP ceramics and preparation method, it is characterised in that：Neodymia and yittrium oxide two oxides are used simultaneously as stable Agent, prepares the nano zirconium oxide powder that two kinds of stabilizers are wrapped up jointly, the powder of synthesis is in atmosphere without pressure using technique for packing Sintering, obtains the tetragonal zirconia polycrystal ceramics with excellent mechanical property.The raw material of use is that mass percent is not less than 99.9 six nitric hydrate neodymium Nd (NO3)3·6H2O, six nitric hydrate yttrium Y (NO3)3·6H2O and average grain size are less than 100 Neodymia molar percentage is in the range of 1.0-2.0 in the monoclinic zirconia powder of nanometer, the TZP ceramics finally obtained, yittrium oxide Molar percentage is in the range of 1.0-1.5.
Chinese patent 200710165634.2 provides a kind of with cubic polycrystal zirconia pottery of the yittrium oxide as stabilizer Porcelain（Y-TZP ceramics）Low-temperature melt producing method, it is mainly characterized by, and includes preparation and the superfine ceramics of precursor sol Prepare two steps：With the soluble-salt containing Mg, Al ion and Si (OC2H5)4For raw material, wherein MgO: Al2O3∶SiO2Mole Than for (0.3-0.8): (2.3-6): precursor sol is made in (1-3.5)；The zirconia nanopowder superfines of stabilized with yttrium oxide is pressed Solid-liquid mass ratio is (75-85): (25-15), which adds water, is made into slurry, addition 3-8wt% precursor sol, uniform mixing and ball milling, Then granulate, be molded, sintered 1-3 hours at 1320-1420 DEG C, obtain nanocrystal Y-TZP ceramics.
Currently available technology is produced using the method for normal sintering, the coarse grains of product, low intensity, it is difficult to for height It is required that high technology ceramics industry.
The content of the invention
High-strength high technology ceramics production purposes can not be met in order to solve prior art, the invention provides a kind of brand-new height Pure high fine and close yttrium stable zirconium oxide ceramics and preparation method thereof.It is an object of the invention to overcome the shortcoming of prior art there is provided High purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof, are made using nanoscale yttrium stable zirconium oxide powder by centrifugal spray The method of grain is granulated, compressing by isostatic cool pressing, is made finally by the method for HIP sintering, present invention tool There is high purity high dense, not only technique and equipment are simple by the present invention, and low cost, high income, energy consumption is low, and production efficiency is high, It is adapted to industrialized production, and results in the tiny controllable yttrium stable zirconium oxide ceramics of steady quality, crystal grain, process of the present invention It is a kind of new low cost, the preparation method of the high purity high dense yttrium stable zirconium oxide ceramics of steady quality without Environment pollution.
The ceramic relative density of high purity high dense yttrium stable zirconium oxide of the present invention is 99% ~ 100%, and host element purity is 99.9% ~ 99.999%, bending strength be 1000 ~ 1600MPa, crystallite dimension be 0.5 ~ 20 micron, Vickers hardness be HV1200 ~ 2000。
Preferably, the relative density of described high purity high dense yttrium stable zirconium oxide ceramics is 99.5% ~ 100%.
Preferably, the host element purity of described high purity high dense yttrium stable zirconium oxide ceramics is 99.99% ~ 99.999%.
Preferably, the bending strength of described high purity high dense yttrium stable zirconium oxide ceramics is 1200 ~ 1600MPa.
Preferably, the crystallite dimension of described high purity high dense yttrium stable zirconium oxide ceramics is 1 ~ 5 micron.
Preferably, the Vickers hardness of described high purity high dense yttrium stable zirconium oxide ceramics is HV1200 ~ 1800.
The host element of high purity high dense yttrium stable zirconium oxide ceramics of the present invention is zirconium oxide, two kinds of yittrium oxide, institute The host element purity stated is the percentage by weight of two kinds of host element weight and gross weight.
In order to reach above-mentioned use requirement, the technical scheme that the present invention is used is high purity high dense yttrium stable zirconium oxide ceramics Preparation method, methods described comprises the following steps that.
（1）Choose high-purity Nano-class and the yttrium stable zirconium oxide powder of specific proportioning.
（2）In step（1）Middle powder is put into binding agent, dispersant and deionized water, carries out ball milling with high energy ball mill, obtains Obtain yttrium stable zirconium oxide powdery pulp.
（3）By step（2）Middle acquisition yttrium stable zirconium oxide powdery pulp, which is put into centrifugal spraying granulator, to be carried out at granulation Reason.
（4）By step（3）The pelletizing of middle acquisition is put into progress isostatic cool pressing processing in isostatic cool pressing gum cover.
（5）By step（4）Middle acquisition isostatic cool pressing blank is put into steel capsule, high temperature insostatic pressing (HIP) jacket is made, jacket is gathered around There are multiple degassing preformed holes.
（6）By step（5）The high temperature insostatic pressing (HIP) jacket of middle acquisition carries out degreasing degassing process.
（7）By step（6）Jacket after the degassing of middle acquisition is put into progress HIP sintering processing in hot isostatic press.
（8）By step（7）The ceramic ingot that middle HIP sintering is finished takes out, and removes jacket, produces high purity high dense Yttrium stable zirconium oxide ceramics.
（9）Measuring process（8）Density, purity, crystallite dimension, bending strength and the hardness of middle yttrium stable zirconium oxide ceramics.
The present invention for high purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof, in order to allow it is of the invention effectively, it is necessary to Above-mentioned steps are refined, specific thinning parameter is as follows.
Step（1）In, the molar percentage of yittrium oxide is 3 ~ 10% in the yttrium stable zirconium oxide powder of selection.
Step（1）In, the primary particle size of described yttrium stable zirconium oxide powder is 1 ~ 100 nanometer.
Step（1）In, the purity of described yttrium stable zirconium oxide powder is 99.9 ~ 99.999%.
Preferably, step（1）In, the molar percentage of yittrium oxide is 3 ~ 5% in the yttrium stable zirconium oxide powder of selection.
Preferably, step（1）In, the yttrium stable zirconium oxide powder primary particle size of selection is 10 ~ 40 nanometers.
Step（2）In, the binding agent of selection includes at least one in polyvinyl alcohol, polyvinyl chloride.
Step（2）In, the dispersant of selection is at least one in ethanol, n-butanol, polyethylene glycol.
Step（2）In, described mixed slurry Ball-milling Time is 2 ~ 12 hours.
Step（2）In, the ball milling ball used by described high energy ball mill is yttrium stable zirconium oxide ball.
Preferably, step（2）In, the binding agent of selection is polyvinyl alcohol.
Preferably, step（2）In, the dispersant of selection is polyethylene glycol.
Preferably, step（2）In, described mixed slurry Ball-milling Time is 4 ~ 8 hours.
Step（3）In, described pelletizing particle diameter is that D50 is 50 ~ 200 microns.
Step（4）In, described isostatic cool pressing gum cover material is one kind in polyurethane, black rubber.
Step（4）In, described isostatic cool pressing processing pressure is 200 ~ 500MPa, and the dwell time is 5 ~ 30 minutes.
Preferably, step（4）In, the isostatic cool pressing gum cover material of selection is polyurethane.
Preferably, step（4）In, the isostatic cool pressing processing pressure of selection is 300 ~ 400MPa, and the dwell time is 10 ~ 15 points Clock.
Step（5）In, described high temperature insostatic pressing (HIP) jacket is welded using argon arc welding.
Step（5）In, the described reserved hole number of high temperature insostatic pressing (HIP) jacket degassing is 1 ~ 50.
Step（6）In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes first stage degassing process, second stage degreasing Processing and phase III degassing process.
Step（6）In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes first stage degassing process parameter for temperature 100 ~ 300 degree, treatment time 2 ~ 24 hours, it is 1.0 × 10-2 ~ 5.0 × 10-2Pa that degassing, which keeps pressure in jacket,.
Step（6）In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes second stage ungrease treatment parameter for temperature 400 ~ 1000 degree, treatment time 2 ~ 48 hours, it is 1.0 × 10-2 ~ 5.0 × 10-2Pa that degassing, which keeps pressure in jacket,.
Step（6）In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes phase III degassing process parameter for temperature 100 ~ 300 degree, treatment time 2 ~ 24 hours, it is 1.0 × 10-3 ~ 5.0 × 10-3Pa that degassing, which keeps pressure in jacket,.
Preferably, step（6）In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes first stage degassing process parameter and is 200 ~ 300 degree of temperature, treatment time 12 ~ 24 hours, it is 1.0 × 10-2 ~ 5.0 × 10-2Pa that degassing, which keeps pressure in jacket,.
Preferably, step（6）In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes second stage ungrease treatment parameter and is 400 ~ 800 degree of temperature, treatment time 12 ~ 24 hours, it is 1.0 × 10-2 ~ 5.0 × 10-2Pa that degassing, which keeps pressure in jacket,.
Preferably, step（6）In, described high temperature insostatic pressing (HIP) jacket degreasing degassing includes phase III degassing process parameter and is 200 ~ 300 degree of temperature, treatment time 12 ~ 24 hours, it is 1.0 × 10-3 ~ 5.0 × 10-3Pa that degassing, which keeps pressure in jacket,.
Step（7）In, described HIP sintering technique is 100 ~ 170MPa of sintering pressure, sintering temperature is 1000 ~ 1400 DEG C, the equalizing temperature time is 0.5 ~ 2 hour, and sintering time is 2 ~ 10 hours.
Preferably, step（7）In, described HIP sintering technique is 140 ~ 170MPa of sintering pressure, sintering temperature For 1100 ~ 1300 DEG C, the equalizing temperature time is 1 ~ 2 hour, and sintering time is 2 ~ 4 hours.
Step（9）In, described density measuring instrument is Archimedes's drainage density of solid detector.
Step（9）In, described purity detecting instrument is inductively coupled plasma atomic emission spectrometer.
Step（9）In, described crystallite dimension measuring instrument is SEM.
Step（9）In, described bending strength measuring instrument measures testing machine for three-point bending.
Step（9）In, described hardness measurement instrument is Vickers.
Step（9）In, the relative density of described yttrium stable zirconium oxide ceramics is 99 ~ 100%.
Step（9）In, the purity of described yttrium stable zirconium oxide ceramics is 99.9 ~ 99.999%.
Step（9）In, the crystallite dimension of described yttrium stable zirconium oxide ceramics is 0.5 ~ 20 micron.
Step（9）In, the bending strength of described yttrium stable zirconium oxide ceramics is 1200 ~ 1600MPa.
Step（9）In, the hardness of described yttrium stable zirconium oxide ceramics is HV1200 ~ 2000.
It is an object of the invention to provide a kind of high purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof, the two of production Zirconia ceramics has the characteristics of high-purity, high densification.
The present invention is a kind of high purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof, compared with prior art, tool Have the advantages that.
（1）By multistage degasification technique, the gaseous impurity content of yttrium stable zirconium oxide ceramics is lower.
（2）By the setting of many stomatas, the internal degassing of yttrium stable zirconium oxide ceramics is more uniform.
（3）By improved heat and other static pressuring processes, the density of yttrium stable zirconium oxide ceramics is higher.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1.
（1）Raw material is selected, the purity of yttrium stable zirconium oxide powder is 99.99%, the molar percentage of yittrium oxide is 3%, one Secondary particle diameter is 17 nanometers, and then powder is put into centrifugal atomizing comminutor again and causes D50 for 121 microns.
（2）The material powder granulated is fitted into progress isostatic cool pressing processing in rubber sleeve, isostatic cool pressing processing pressure is 360MPa, the dwell time is 10 minutes.
（3）The blank suppressed is fitted into steel capsule, steel capsule reserves 16 stomatas.
（4）It is 200 DEG C that steel capsule is carried out into a stage degassing temperature, and degassing time is 12 hours, and the pressure in jacket is 1.0×10-2Pa；Two-stage skimming temp is 600 DEG C, and degreasing time is 24 hours, and the pressure in jacket is 1.0 × 10-2Pa； Three stage degassing temperatures are 200 DEG C, and degassing time is 12 hours, and the pressure in jacket is 1.0 × 10-3Pa, then by all gas Shut in hole.
（5）The jacket manufactured is placed in hot isostatic press and carries out HIP sintering, HIP sintering parameter, temperature 1250 degree of degree, sintering pressure is 170MPa, and the equalizing temperature time is 1 hour, and sintering time is 4 hours.
（6）Jacket is removed, ceramic ingot is cut into specified yttrium stable zirconium oxide ceramic shape.
（7）The relative density for measuring yttrium stable zirconium oxide ceramics is that 99.8%, purity is that 99.9912%, crystallite dimension is 1.1 Micron, hardness are HV1371, and bending strength is 1489MPa.
Embodiment 2.
（1）Raw material is selected, the purity of yttrium stable zirconium oxide powder is 99.995%, the molar percentage of yittrium oxide is 5%, one Secondary particle diameter is 35 nanometers, and then powder is put into centrifugal atomizing comminutor again and causes D50 for 142 microns.
（2）The material powder granulated is fitted into progress isostatic cool pressing processing in rubber sleeve, isostatic cool pressing processing pressure is 380MPa, the dwell time is 12 minutes.
（3）The blank suppressed is fitted into steel capsule, steel capsule reserves 24 stomatas.
（4）It is 240 DEG C that steel capsule is carried out into a stage degassing temperature, and degassing time is 18 hours, and the pressure in jacket is 1.0×10-2Pa；Two-stage skimming temp is 650 DEG C, and degreasing time is 28 hours, and the pressure in jacket is 1.0 × 10-2Pa； Three stage degassing temperatures are 220 DEG C, and degassing time is 16 hours, and the pressure in jacket is 1.0 × 10-3Pa, then by all gas Shut in hole.
（5）The jacket manufactured is placed in hot isostatic press and carries out HIP sintering, HIP sintering parameter, temperature 1300 degree of degree, sintering pressure is 157MPa, and the equalizing temperature time is 1 hour, and sintering time is 5 hours.
（6）Jacket is removed, ceramic ingot is cut into specified yttrium stable zirconium oxide ceramic shape.
（7）The relative density for measuring yttrium stable zirconium oxide ceramics is that 99.6%, purity is that 99.9949%, crystallite dimension is 1.8 Micron, hardness are HV1328, and bending strength is 1356MPa.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all according to the present invention The equivalent change or modification that Spirit Essence is made, should all cover within the scope of the present invention.

Claims (10)

1. a kind of high purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof, it is characterised in that comprise the following steps that：
（1）Choose high-purity Nano-class and the yttrium stable zirconium oxide powder of specific proportioning；
（2）In step（1）Middle powder is put into binding agent, dispersant and deionized water, and ball milling is carried out with high energy ball mill, obtains yttrium Oxide-stabilizing zirconia powder slurry；
（3）By step（2）Middle acquisition yttrium stable zirconium oxide powdery pulp is put into progress granulation processing in centrifugal spraying granulator；
（4）By step（3）The pelletizing of middle acquisition is put into progress isostatic cool pressing processing in isostatic cool pressing gum cover；
（5）By step（4）Middle acquisition isostatic cool pressing blank is put into steel capsule, and high temperature insostatic pressing (HIP) jacket is made；
（6）By step（5）The high temperature insostatic pressing (HIP) jacket of middle acquisition carries out degreasing degassing process；
（7）By step（6）Jacket after the degassing of middle acquisition is put into progress HIP sintering processing in hot isostatic press；
（8）By step（7）The ceramic ingot that middle HIP sintering is finished takes out, and removes jacket, produces high purity high dense yttrium steady Determine zirconia ceramics；
（9）Measuring process（8）Density, purity, crystallite dimension, bending strength and the hardness of middle yttrium stable zirconium oxide ceramics.
2. high purity high dense yttrium stable zirconium oxide ceramics according to claim 1 and preparation method thereof, it is characterised in that：Step Suddenly（1）In, the molar percentage of yittrium oxide is 3 ~ 10% in described yttrium stable zirconium oxide powder.
3. high purity high dense yttrium stable zirconium oxide ceramics according to claim 1 and preparation method thereof, it is characterised in that：Step Suddenly（1）In, the primary particle size of described yttrium stable zirconium oxide powder is 1 ~ 100 nanometer.
4. high purity high dense yttrium stable zirconium oxide ceramics according to claim 1 and preparation method thereof, it is characterised in that：Step Suddenly（1）In, the purity of described yttrium stable zirconium oxide powder is 99.9 ~ 99.999%.
5. high purity high dense yttrium stable zirconium oxide ceramics according to claim 1 and preparation method thereof, it is characterised in that：Step Suddenly（7）In, described sintering method is HIP sintering.
6. high purity high dense yttrium stable zirconium oxide ceramics according to claim 1 and preparation method thereof, it is characterised in that：Step Suddenly（9）In, the relative density of described yttrium stable zirconium oxide ceramics is 99 ~ 100%.
7. high purity high dense yttrium stable zirconium oxide ceramics according to claim 1 and preparation method thereof, it is characterised in that：Step Suddenly（9）In, the purity of described yttrium stable zirconium oxide ceramics is 99.9 ~ 99.999%.
8. high purity high dense yttrium stable zirconium oxide ceramics according to claim 1 and preparation method thereof, it is characterised in that：Step Suddenly（9）In, the crystallite dimension of described yttrium stable zirconium oxide ceramics is 0.5 ~ 20 micron.
9. high purity high dense yttrium stable zirconium oxide ceramics according to claim 1 and preparation method thereof, it is characterised in that：Step Suddenly（9）In, the bending strength of described yttrium stable zirconium oxide ceramics is 1200 ~ 1600MPa.
10. high purity high dense yttrium stable zirconium oxide ceramics according to claim 1 and preparation method thereof, it is characterised in that： Step（9）In, the hardness of described yttrium stable zirconium oxide ceramics is HV1200 ~ 2000.
CN201710144563.1A 2017-03-13 2017-03-13 High purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof Pending CN106938931A (en)

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