CN110104681A - A kind of high-ductility stabilized with yttrium oxide tetragonal zircite material and preparation method thereof not influenced by sintering - Google Patents
A kind of high-ductility stabilized with yttrium oxide tetragonal zircite material and preparation method thereof not influenced by sintering Download PDFInfo
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- CN110104681A CN110104681A CN201910367294.4A CN201910367294A CN110104681A CN 110104681 A CN110104681 A CN 110104681A CN 201910367294 A CN201910367294 A CN 201910367294A CN 110104681 A CN110104681 A CN 110104681A
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- 239000000463 material Substances 0.000 title claims abstract description 69
- 238000005245 sintering Methods 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 title claims abstract description 20
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000007858 starting material Substances 0.000 claims abstract description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 32
- 229910052593 corundum Inorganic materials 0.000 claims description 25
- 239000010431 corundum Substances 0.000 claims description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims description 19
- 229920001223 polyethylene glycol Polymers 0.000 claims description 19
- 238000013019 agitation Methods 0.000 claims description 18
- 239000000654 additive Substances 0.000 claims description 14
- 230000000996 additive effect Effects 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000004615 ingredient Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000000889 atomisation Methods 0.000 claims description 9
- 238000000748 compression moulding Methods 0.000 claims description 9
- 239000004570 mortar (masonry) Substances 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 235000005979 Citrus limon Nutrition 0.000 claims 2
- 244000248349 Citrus limon Species 0.000 claims 1
- 244000131522 Citrus pyriformis Species 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 17
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000919 ceramic Substances 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- GBNDTYKAOXLLID-UHFFFAOYSA-N zirconium(4+) ion Chemical compound [Zr+4] GBNDTYKAOXLLID-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 17
- 238000001228 spectrum Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 9
- 229910021645 metal ion Inorganic materials 0.000 description 8
- 238000009738 saturating Methods 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 8
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 7
- 229910003101 Y(NO3)3·6H2O Inorganic materials 0.000 description 7
- 238000007088 Archimedes method Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 244000137852 Petrea volubilis Species 0.000 description 5
- 229910003978 SiClx Inorganic materials 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000007373 indentation Methods 0.000 description 5
- 238000005498 polishing Methods 0.000 description 5
- 238000007545 Vickers hardness test Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005118 spray pyrolysis Methods 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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- 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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
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- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B2235/3246—Stabilised zirconias, e.g. YSZ or cerium stabilised zirconia
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Abstract
The present invention relates to high-ductility stabilized with yttrium oxide tetragonal zircite materials not influenced by sintering and preparation method thereof, belong to zirconia ceramics field.A kind of high-ductility stabilized with yttrium oxide tetragonal zircite (3Y-TZP) material not influenced by sintering, particle size is between 100nm-900nm, no monoclinic phase, sintered density 5.63g/cm3‑6.05g/cm3, relative density 92.6%-99.5%.For the present invention compared with similar technique, the present invention makes raw material reaction uniformly from atomic scale, avoids zirconium ion from hydrolyzing, so starting material is just without monoclinic phase；1350-1550 DEG C of range of sintering temperature is wider, keeps sintering process simple；Toughness is relatively high, and does not have significant decrease with sintering time and temperature.
Description
Technical field
The present invention relates to high-ductility stabilized with yttrium oxide tetragonal zircite materials not influenced by sintering and preparation method thereof, belong to
Zirconia ceramics field.
Background technique
The yttrium partially stabilized tetragonal zircite of oxidation (3Y-TZP) material that molar fraction is 3% is because having high-melting-point, low-heat
The features such as conductance, high intensity, high tenacity, corrosion-resistant and excellent chemical stability, especially there is good mechanical property,
If bending strength reaches 1000MPa, fracture toughness is up to 3.0-6.5MPam1/2, in machinery, electronics, petroleum, chemical industry, aviation, boat
It, weaving, the industries such as precision instrument and medical treatment all have a wide range of applications.
The preparation of conventional high-temperature sintering process is close to complete fully dense 3Y-TZP ceramics vulnerable to ZrO2The intrinsic thermodynamics of substrate
The limitation of Phase-change Problems.According to ZrO2-Y2O3Phasor, 3Y-TZP have metastable tetragonal zirconia (t') phase structure at room temperature.T' phase is heat
Mechanics is instable, 1200 DEG C or more at a temperature of experience by diffusion control four directions (t) mutually and cube (c) phase transition, t
It mutually can be further transformed to monoclinic crystal (m) phase (- 1170 DEG C) while cooling.Well-known ZrO2In from t phase to the geneva of m phase
Body phase transformation along with -4Vol% volume expansion.The stress that this volume change generates, which can lead to, forms crackle in ceramics, in turn
Cause the cracking of component even broken.So domestic and foreign scholars generally use the Fast Sinterings techniques such as discharge plasma sintering
Fine and close t'-YSZ block is prepared, to avoid fragmentation ceramic in sintering process.
Currently, hydrothermal synthesis method and co-precipitation legal system is usually used in reported in the literature and commercialized 3Y-TZP powder
It is standby.Since the 3Y- that hydrolysis reduces the uniformity of metal ion in solution distribution, and then the above method is caused to prepare easily occurs for zirconates
TZP powder contains a small amount of monoclinic phase.Starting powder in monoclinic phase appearance not only result in 3Y-TZP material fracture it is tough
Property reduce, while also increasing 3Y-TZP ceramics chipping risk during the sintering process, make its sintering process parameter range
Become very narrow.Therefore it provides a kind of phase purity is high, without the adaptable 3Y-TZP material of monoclinic phase and sintering process and its system
Preparation Method will greatly improve the quality and reliability of zirconium oxide ceramic component, be its application in high performance structure ceramic field
Play great facilitation.
Summary of the invention
Present invention aim to address above-mentioned zirconium oxides (3Y-TZP) there are monoclinic phase, and the narrow deficiency of sintering range is asked
Topic provides a kind of high-ductility stabilized with yttrium oxide tetragonal zircite (3Y-TZP) material and preparation method thereof not influenced by sintering.It should
Material is single tetragonal zircite structure, and for crystallite dimension between 10nm-40nm, which is to utilize Sol- spray pyrolysis
Method and be made.
Used technical solution is the present invention in order to solve the above problem: the high-ductility yttrium oxide that one kind is not influenced by sintering is steady
Determine tetragonal zircite (3Y-TZP) material, particle size is between 100nm-900nm, sintered density 5.63g/cm3-
6.05g/cm3, relative density 92.6%-99.5%.
According to the present invention, a kind of high-ductility stabilized with yttrium oxide tetragonal zircite (3Y-TZP) material not influenced by sintering is provided
The preparation method of material, characterized in that it comprises the following steps:
(1) colloidal sol is prepared:
Zr (NO3) 43H2O:Y (NO3) 36H2O=0.94:0.06 ingredient in molar ratio, is configured to transparent aqueous solution；
Doping citric acid and polyethylene glycol again, the colloidal sol of magnetic agitation to clear；
(2) prepared by raw material:
Using the pure air of certain pressure as atomizing medium, above-mentioned prepared colloidal sol is atomised to corundum crucible；Atomization
After temperature risen into certain temperature be again heat-treated to obtain required raw material, warm sintering is cooled to room temperature after 1 hour
Obtain 3Y-TZP nanometer powder；
(3) prepared by bulk:
After above-mentioned 3Y-TZP nanometer powder is milled, disk is pressed into mold is put into program-controlled high temperature furnace sintering and be prepared into
Disk.
The preparation method of high-ductility stabilized with yttrium oxide tetragonal zircite (3Y-TZP) material that described one kind is not influenced by sintering,
It is characterized in that, (1) the colloidal sol preparation:
It is described to press material molar ratio ingredient: Zr (NO3) 43H2O:Y (NO3) 36H2O=0.94:0.06；With deionization
Water is solvent, preparing metal total ion concentration be 0.2 you/liter aqueous solution；Sequentially add additive citric acid and poly- second two
Alcohol, citric acid additive amount are 160g/L, molecular weight polyethylene glycol 20000, additive amount 20g/L；Magnetic agitation is saturating to clarifying
It is bright.
(2) raw material preparation: using purity for 99.99% air is atomizing medium, pressure 0.3MPa；Corundum
Crucible temperature is 500 DEG C -900 DEG C.
(3) the bulk preparation: the 3Y-TZP material is to be with the 3Y-TZP nanometer powder after 900 DEG C of heat treatment 1h
Beginning raw material, puts the powder into agate mortar and mills, and takes and is put into the stainless steel mould that diameter is 18mm in right amount,
Molding disk is put into program-controlled high temperature furnace in 1350 DEG C of -1600 DEG C of sintering 1.5-2.5h by compression moulding under 500MPa pressure,
Temperature rate is 2 DEG C/min, is prepared into after being cooled to room temperature with a thickness of 2mm disk.
According to the present invention, the 3Y-TZP nanometer powder is after 1350 DEG C of -1600 DEG C of sintering 2h, above-mentioned 3Y-TZP material
There is not any monoclinic zirconia diffraction maximum to occur in XRD spectrum.
The present invention has substantive distinguishing features outstanding compared with similar technique:
1. its appearance not only results in the fracture of 3Y-TZP material because having monoclinic phase in general merchandiseization starting powder
Toughness reduces, while also increasing 3Y-TZP ceramics chipping risk during the sintering process, makes its sintering process parameter model
Enclosing becomes very narrow.Our providing methods make raw material reaction uniformly from atomic scale, avoid zirconium ion from hydrolyzing, so starting material is just
There is no monoclinic phase.
2. sintering range is wider, 1350-1550, keep sintering process simple；
3. toughness is relatively high, and does not have significant decrease with sintering time and temperature.
Detailed description of the invention
Fig. 1 is the nanometer 3Y-TZP powder of embodiment according to the present invention preparation after 500 DEG C of -900 DEG C of heat treatment 1h
XRD spectrum；What is provided together in figure is the standard PDF card map (number: PDF#881007) of tetragonal zircite；Crystal grain in figure
Dimension D is peak position θ, halfwidth β and X-ray wavelength λ=0.15406nm based on (111) crystallographic plane diffraction peak, using Scherrer public affairs
Formula: D=0.89 λ/β cos θ is calculated.
Fig. 2 is the XRD spectrum of the 3Y-TZP material of embodiment according to the present invention preparation.
Fig. 3 (a), 3 (b) 3 (c), 3 (d), 3 (e) and 3 (f) are the 3Y-TZP material of embodiment according to the present invention preparation respectively
The surface SEM image of material.
The measurement density and theoretical density that Fig. 4 is the 3Y-TZP material of embodiment according to the present invention preparation are with sintering temperature
Variation relation figure.
Fig. 5 (a), 5 (b) 5 (c), 5 (d) and 5 (e) are that the 3Y-TZP material of embodiment according to the present invention preparation is thrown respectively
The SEM image (load p=9.8N, dwell time t=10s) of the Vickers indentation of optical surface.
The fracture toughness and Vickers hardness that Fig. 6 is the 3Y-TZP material of embodiment according to the present invention preparation are with sintering temperature
Variation relation figure.
Specific embodiment
According to an aspect of the invention, there is provided a kind of high-ductility stabilized with yttrium oxide tetragonal zircite not influenced by sintering
Material, in which:
The 3Y-TZP nanometer powder is prepared using colloidal sol-spray pyrolysis,
The 3Y-TZP nanometer powder is through the following steps that be made:
Zr (the NO for being 99.99% with purity3)4·3H2O and Y (NO3)3·6H2O is raw material, in molar ratio Zr (NO3)4·
3H2O:Y(NO3)3·6H2O=0.94:0.06 ingredient, using deionized water as solvent, being configured to metal ion total concentration is
The aqueous solution of 0.2mol/L after magnetic agitation 1-3h to clear, sequentially adds six water citric acid of additive and molecular weight
For 20000 polyethylene glycol, wherein citric acid adding amount 160g/L, polyethylene glycol 20g/L, then it is saturating to clarifying through magnetic agitation
It is bright, so that colloidal sol be made.
Above-mentioned prepared colloidal sol is atomised in corundum crucible using pressure atomization method, atomizing pressure 0.3MPa,
Corundum crucible temperature is 500 DEG C.After colloidal sol is atomized, corundum crucible temperature is risen into 500 DEG C -900 DEG C (100 DEG C of intervals) and is protected
It is cooled to room temperature after warm 1h and obtains 3Y-TZP nanometer powder.
According to another aspect of the present invention, above-mentioned 3Y-TZP nanometer powder is after 500 DEG C of -900 DEG C of heat treatment 1h
Single tetragonal zircite structure.
According to another aspect of the present invention, crystalline substance of the above-mentioned 3Y-TZP nanometer powder after 500 DEG C of -900 DEG C of heat treatment 1h
Particle size is between 10nm-40nm.
A specific aspect according to the present invention, above-mentioned 3Y-TZP material are received with the 3Y-TZP after 900 DEG C of heat treatment 1h
Rice flour end is starting material, puts the powder into agate mortar and mills, and takes the stainless steel mold for being put into that diameter is 18mm in right amount
In tool, molding disk is put into program-controlled high temperature furnace in 1350 DEG C -1600 DEG C (intervals by the compression moulding under 500MPa pressure
50 DEG C) sintering 2h, temperature rate is 2 DEG C/min, is prepared into after being cooled to room temperature with a thickness of 2mm disk.
Another specific aspect according to the present invention, after 1350 DEG C of -1600 DEG C of sintering 2h, above-mentioned 3Y-TZP material
There is not any monoclinic zirconia diffraction maximum to occur in XRD spectrum.
Another specific aspect according to the present invention, the particle size of above-mentioned 3Y-TZP material between 100nm-900nm it
Between, sintered density 5.63g/cm3-6.05g/cm3, relative density 92.6%-99.5%.
Another specific aspect according to the present invention tests the fracture toughness of above-mentioned 3Y-TZP material using Vickers indentation method
For in 3.94MPm1/2-4.98MP·m1/2In range, hardness is between 6.61GPa-11.54GPa.
Below in conjunction with drawings and examples, the present invention is described in further detail.
Embodiment 1:
Zr (the NO for being 99.99% with purity3)4·3H2O and Y (NO3)3·6H2O is raw material, in molar ratio Zr (NO3)4·
3H2O:Y(NO3)3·6H2O=0.94:0.06 ingredient, using deionized water as solvent, being configured to metal ion total concentration is
The aqueous solution of 0.2mol/L after magnetic agitation 1-3h to clear, sequentially adds six water citric acid of additive and molecular weight
For 20000 polyethylene glycol, wherein citric acid adding amount 160g/L, polyethylene glycol 20g/L, then it is saturating to clarifying through magnetic agitation
It is bright, so that colloidal sol be made.
Above-mentioned prepared colloidal sol is atomised in corundum crucible using pressure atomization method, atomizing pressure 0.3MPa,
Corundum crucible temperature is 500 DEG C.After colloidal sol is atomized, it is cooled to room temperature after corundum crucible temperature is risen to 900 DEG C of heat preservation 1h
Obtain 3Y-TZP nanometer powder.
It puts the powder into agate mortar and mills, take and be put into the stainless steel mould that diameter is 18mm in right amount,
Molding disk is put into program-controlled high temperature furnace in 1350 DEG C of sintering 2h, temperature rate 2 by compression moulding under 500MPa pressure
DEG C/min, it is prepared into after being cooled to room temperature with a thickness of 2mm disk, for test.
Using model X ' Pert PRO of Dutch Panaco company production, it is furnished with the super detector of X ' Celerator
Multi-functional X ray diffractometer carries out object and mutually tests, and x-ray is Cu target k α 1, wavelength X=0.15406nm.Its XRD spectrum refers to
1# in Fig. 2.3Y-TZP is observed using the field emission scanning electron microscope of the model Ultra 55 of Zeiss, Germany company production
The particle size of material is 185 ± 50nm, and SEM image refers to Fig. 3 (a).
The theoretical density ρ of material is calculated according to XRD data and chemical componentt=6.08g/cm3, surveyed using Archimedes method
Try disk density ρ=5.63g/cm3, material relative density ρ is calculated according to formula (1)r=92.6%, refer to Fig. 4.
ρr=ρ/ρt× 100% (1)
Embodiment 2:
Zr (the NO for being 99.99% with purity3)4·3H2O and Y (NO3)3·6H2O is raw material, in molar ratio Zr (NO3)4·
3H2O:Y(NO3)3·6H2O=0.94:0.06 ingredient, using deionized water as solvent, being configured to metal ion total concentration is
The aqueous solution of 0.2mol/L after magnetic agitation 1-3h to clear, sequentially adds six water citric acid of additive and molecular weight
For 20000 polyethylene glycol, wherein citric acid adding amount 160g/L, polyethylene glycol 20g/L, then it is saturating to clarifying through magnetic agitation
It is bright, so that colloidal sol be made.
Above-mentioned prepared colloidal sol is atomised in corundum crucible using pressure atomization method, atomizing pressure 0.3MPa,
Corundum crucible temperature is 500 DEG C.After colloidal sol is atomized, it is cooled to room temperature after corundum crucible temperature is risen to 900 DEG C of heat preservation 1h
Obtain 3Y-TZP nanometer powder.
It puts the powder into agate mortar and mills, take and be put into the stainless steel mould that diameter is 18mm in right amount,
Molding disk is put into program-controlled high temperature furnace in 1400 DEG C of sintering 2h, temperature rate 2 by compression moulding under 500MPa pressure
DEG C/min, it is prepared into after being cooled to room temperature with a thickness of 2mm disk, for test.
Using model X ' Pert PRO of Dutch Panaco company production, it is furnished with the super detector of X ' Celerator
Multi-functional X ray diffractometer carries out object and mutually tests, and x-ray is Cu target k α 1, wavelength X=0.15406nm.Its XRD spectrum refers to
2# in Fig. 2.3Y-TZP is observed using the field emission scanning electron microscope of the model Ultra 55 of Zeiss, Germany company production
The particle size of material is 234 ± 69nm, and SEM image refers to Fig. 3 (b).
The theoretical density ρ of material is calculated according to XRD data and chemical componentt=6.08g/cm3, surveyed using Archimedes method
Try disk density ρ=5.88g/cm3, material relative density ρ is calculated according to formula (1)r=96.7%, refer to Fig. 4.Using carbon
After SiClx sand paper carries out surface polishing treatment to 3Y-TZP material, the model of Beijing epoch mountain peak Science and Technology Ltd. production is utilized
Impression test, ram load P=9.8N, dwell time t=10s are carried out for the Vickers of HVS -30Z, indentation image is asked
Referring to Fig. 5 (a), and according to the hardness H of formula (2) calculating materialV=6.61 ± 0.16GPa calculates material according to formula (3)
Fracture toughness KIC=3.94 ± 0.16MPam1/2, refer to Fig. 6.
HV=P/2a2 (2)
KIC=0.16HV·a1/2·(c/a)-3/2(c/a≥2.5)(3)
Embodiment 3:
Zr (the NO for being 99.99% with purity3)4·3H2O and Y (NO3)3·6H2O is raw material, in molar ratio Zr (NO3)4·
3H2O:Y(NO3)3·6H2O=0.94:0.06 ingredient, using deionized water as solvent, being configured to metal ion total concentration is
The aqueous solution of 0.2mol/L after magnetic agitation 1-3h to clear, sequentially adds six water citric acid of additive and molecular weight
For 20000 polyethylene glycol, wherein citric acid adding amount 160g/L, polyethylene glycol 20g/L, then it is saturating to clarifying through magnetic agitation
It is bright, so that colloidal sol be made.
Above-mentioned prepared colloidal sol is atomised in corundum crucible using pressure atomization method, atomizing pressure 0.3MPa,
Corundum crucible temperature is 500 DEG C.After colloidal sol is atomized, it is cooled to room temperature after corundum crucible temperature is risen to 900 DEG C of heat preservation 1h
Obtain 3Y-TZP nanometer powder.
It puts the powder into agate mortar and mills, take and be put into the stainless steel mould that diameter is 18mm in right amount,
Molding disk is put into program-controlled high temperature furnace in 1450 DEG C of sintering 2h, temperature rate 2 by compression moulding under 500MPa pressure
DEG C/min, it is prepared into after being cooled to room temperature with a thickness of 2mm disk, for test.
Using model X ' Pert PRO of Dutch Panaco company production, it is furnished with the super detector of X ' Celerator
Multi-functional X ray diffractometer carries out object and mutually tests, and x-ray is Cu target k α 1, wavelength X=0.15406nm.Its XRD spectrum refers to
3# in Fig. 2.3Y-TZP is observed using the field emission scanning electron microscope of the model Ultra 55 of Zeiss, Germany company production
The particle size of material is 269 ± 65nm, and SEM image refers to Fig. 3 (c).
The theoretical density ρ of material is calculated according to XRD data and chemical componentt=6.08g/cm3, surveyed using Archimedes method
Try disk density ρ=5.95g/cm3, material relative density ρ is calculated according to formula (1)r=97.9%, refer to Fig. 4.Using carbon
After SiClx sand paper carries out surface polishing treatment to 3Y-TZP material, the model of Beijing epoch mountain peak Science and Technology Ltd. production is utilized
Impression test, ram load P=9.8N, dwell time t=10s are carried out for the Vickers of HVS -30Z, indentation image is asked
Referring to Fig. 5 (b), and according to the hardness H of formula (2) calculating materialV=10.10 ± 0.30GPa calculates material according to formula (3)
Fracture toughness KIC=4.26 ± 0.26MPam1/2, refer to Fig. 6.
Embodiment 4:
Zr (the NO for being 99.99% with purity3)4·3H2O and Y (NO3)3·6H2O is raw material, in molar ratio Zr (NO3)4·
3H2O:Y(NO3)3·6H2O=0.94:0.06 ingredient, using deionized water as solvent, being configured to metal ion total concentration is
The aqueous solution of 0.2mol/L after magnetic agitation 1-3h to clear, sequentially adds six water citric acid of additive and molecular weight
For 20000 polyethylene glycol, wherein citric acid adding amount 160g/L, polyethylene glycol 20g/L, then it is saturating to clarifying through magnetic agitation
It is bright, so that colloidal sol be made.
Above-mentioned prepared colloidal sol is atomised in corundum crucible using pressure atomization method, atomizing pressure 0.3MPa,
Corundum crucible temperature is 500 DEG C.After colloidal sol is atomized, it is cooled to room temperature after corundum crucible temperature is risen to 900 DEG C of heat preservation 1h
Obtain 3Y-TZP nanometer powder.
It puts the powder into agate mortar and mills, take and be put into the stainless steel mould that diameter is 18mm in right amount,
Molding disk is put into program-controlled high temperature furnace in 1500 DEG C of sintering 2h, temperature rate 2 by compression moulding under 500MPa pressure
DEG C/min, it is prepared into after being cooled to room temperature with a thickness of 2mm disk, for test.
Using model X ' Pert PRO of Dutch Panaco company production, it is furnished with the super detector of X ' Celerator
Multi-functional X ray diffractometer carries out object and mutually tests, and x-ray is Cu target k α 1, wavelength X=0.15406nm.Its XRD spectrum refers to
4# in Fig. 2.3Y-TZP is observed using the field emission scanning electron microscope of the model Ultra 55 of Zeiss, Germany company production
The particle size of material is 321 ± 91nm, and SEM image refers to Fig. 3 (d).
The theoretical density ρ of material is calculated according to XRD data and chemical componentt=6.08g/cm3, surveyed using Archimedes method
Try disk density ρ=5.98g/cm3, material relative density ρ is calculated according to formula (1)r=98.4%, refer to Fig. 4.Using carbon
After SiClx sand paper carries out surface polishing treatment to 3Y-TZP material, the model of Beijing epoch mountain peak Science and Technology Ltd. production is utilized
Impression test, ram load P=9.8N, dwell time t=10s are carried out for the Vickers of HVS -30Z, indentation image is asked
Referring to Fig. 5 (c), and according to the hardness H of formula (2) calculating materialV=10.35 ± 0.37GPa calculates material according to formula (3)
Fracture toughness KIC=4.13 ± 0.22MPam1/2, refer to Fig. 6.
Embodiment 5:
Zr (the NO for being 99.99% with purity3)4·3H2O and Y (NO3)3·6H2O is raw material, in molar ratio Zr (NO3)4·
3H2O:Y(NO3)3·6H2O=0.94:0.06 ingredient, using deionized water as solvent, being configured to metal ion total concentration is
The aqueous solution of 0.2mol/L after magnetic agitation 1-3h to clear, sequentially adds six water citric acid of additive and molecular weight
For 20000 polyethylene glycol, wherein citric acid adding amount 160g/L, polyethylene glycol 20g/L, then it is saturating to clarifying through magnetic agitation
It is bright, so that colloidal sol be made.
Above-mentioned prepared colloidal sol is atomised in corundum crucible using pressure atomization method, atomizing pressure 0.3MPa,
Corundum crucible temperature is 500 DEG C.After colloidal sol is atomized, it is cooled to room temperature after corundum crucible temperature is risen to 900 DEG C of heat preservation 1h
Obtain 3Y-TZP nanometer powder.
It puts the powder into agate mortar and mills, take and be put into the stainless steel mould that diameter is 18mm in right amount,
Molding disk is put into program-controlled high temperature furnace in 1550 DEG C of sintering 2h, temperature rate 2 by compression moulding under 500MPa pressure
DEG C/min, it is prepared into after being cooled to room temperature with a thickness of 2mm disk, for test.
Using model X ' Pert PRO of Dutch Panaco company production, it is furnished with the super detector of X ' Celerator
Multi-functional X ray diffractometer carries out object and mutually tests, and x-ray is Cu target k α 1, wavelength X=0.15406nm.Its XRD spectrum refers to
5# in Fig. 2.3Y-TZP is observed using the field emission scanning electron microscope of the model Ultra 55 of Zeiss, Germany company production
The particle size of material is 506 ± 133nm, and SEM image refers to Fig. 3 (e).
The theoretical density ρ of material is calculated according to XRD data and chemical componentt=6.08g/cm3, surveyed using Archimedes method
Try disk density ρ=6.03g/cm3, material relative density ρ is calculated according to formula (1)r=99.2%, refer to Fig. 4.Using carbon
After SiClx sand paper carries out surface polishing treatment to 3Y-TZP material, the model of Beijing epoch mountain peak Science and Technology Ltd. production is utilized
Impression test, ram load P=9.8N, dwell time t=10s are carried out for the Vickers of HVS -30Z, indentation image is asked
Referring to Fig. 5 (d), and according to the hardness H of formula (2) calculating materialV=11.52 ± 0.11GPa calculates material according to formula (3)
Fracture toughness KIC=4.30 ± 0.21MPam1/2, refer to Fig. 6.
Embodiment 6:
Zr (the NO for being 99.99% with purity3)4·3H2O and Y (NO3)3·6H2O is raw material, in molar ratio Zr (NO3)4·
3H2O:Y(NO3)3·6H2O=0.94:0.06 ingredient, using deionized water as solvent, being configured to metal ion total concentration is
The aqueous solution of 0.2mol/L after magnetic agitation 1-3h to clear, sequentially adds six water citric acid of additive and molecular weight
For 20000 polyethylene glycol, wherein citric acid adding amount 160g/L, polyethylene glycol 20g/L, then it is saturating to clarifying through magnetic agitation
It is bright, so that colloidal sol be made.
Above-mentioned prepared colloidal sol is atomised in corundum crucible using pressure atomization method, atomizing pressure 0.3MPa,
Corundum crucible temperature is 500 DEG C.After colloidal sol is atomized, it is cooled to room temperature after corundum crucible temperature is risen to 900 DEG C of heat preservation 1h
Obtain 3Y-TZP nanometer powder.
It puts the powder into agate mortar and mills, take and be put into the stainless steel mould that diameter is 18mm in right amount,
Molding disk is put into program-controlled high temperature furnace in 1600 DEG C of sintering 2h, temperature rate 2 by compression moulding under 500MPa pressure
DEG C/min, it is prepared into after being cooled to room temperature with a thickness of 2mm disk, for test.
Using model X ' Pert PRO of Dutch Panaco company production, it is furnished with the super detector of X ' Celerator
Multi-functional X ray diffractometer carries out object and mutually tests, and x-ray is Cu target k α 1, wavelength X=0.15406nm.Its XRD spectrum refers to
6# in Fig. 2.3Y-TZP is observed using the field emission scanning electron microscope of the model Ultra 55 of Zeiss, Germany company production
The particle size of material is 709 ± 170nm, and SEM image refers to Fig. 3 (f).
The theoretical density ρ of material is calculated according to XRD data and chemical componentt=6.08g/cm3, surveyed using Archimedes method
Try disk density ρ=6.05g/cm3, material relative density ρ is calculated according to formula (1)r=99.5%, refer to Fig. 4.Using carbon
After SiClx sand paper carries out surface polishing treatment to 3Y-TZP material, the model of Beijing epoch mountain peak Science and Technology Ltd. production is utilized
Impression test, ram load P=9.8N, dwell time t=10s are carried out for the Vickers of HVS -30Z, indentation image is asked
Referring to Fig. 5 (e), and according to the hardness H of formula (2) calculating materialV=11.54 ± 0.13GPa calculates material according to formula (3)
Fracture toughness KIC=4.98 ± 0.38MPam1/2, refer to Fig. 6.
Claims (5)
1. high-ductility stabilized with yttrium oxide tetragonal zircite (3Y-TZP) material that one kind is not influenced by sintering, which is characterized in that particle
Size is between 100nm-900nm, no monoclinic phase, sintered density 5.63g/cm3-6.05g/cm3, relative density 92.6%-
99.5%.
2. high-ductility stabilized with yttrium oxide tetragonal zircite (3Y-TZP) material that one kind described in claim 1 is not influenced by sintering
Preparation method, characterized in that it comprises the following steps:
(1) colloidal sol is prepared:
Zr (NO3) 43H2O:Y (NO3) 36H2O=0.94:0.06 ingredient in molar ratio, is configured to transparent aqueous solution；Again plus
Additive citric acid and polyethylene glycol, the colloidal sol of magnetic agitation to clear；
(2) prepared by raw material:
Using the pure air of certain pressure as atomizing medium, above-mentioned prepared colloidal sol is atomised to corundum crucible；Atomization finishes
Temperature is risen to certain temperature again afterwards to be heat-treated to obtain required raw material, warm sintering was cooled to room temperature acquisition after 1 hour
3Y-TZP nanometer powder；
(3) prepared by bulk:
After above-mentioned 3Y-TZP nanometer powder is milled, disk is pressed into mold is put into program-controlled high temperature furnace sintering and be prepared into circle
Piece.
3. high-ductility stabilized with yttrium oxide tetragonal zircite (3Y-TZP) material that one kind as claimed in claim 2 is not influenced by sintering
Preparation method, which is characterized in that (1) the colloidal sol preparation:
It is described to press material molar ratio ingredient: Zr (NO3) 43H2O:Y (NO3) 36H2O=0.94:0.06；It is with deionized water
Solvent, preparing metal total ion concentration be 0.2 you/liter aqueous solution；Sequentially add additive citric acid and polyethylene glycol, lemon
Lemon acid additive amount is 160g/L, molecular weight polyethylene glycol 20000, additive amount 20g/L；Magnetic agitation is to clear.
4. high-ductility stabilized with yttrium oxide tetragonal zircite (3Y-TZP) material that one kind as claimed in claim 2 is not influenced by sintering
Preparation method, which is characterized in that (2) raw material preparation: using purity for 99.99% air is atomizing medium,
Pressure is 0.3MPa；Corundum crucible temperature is 500 DEG C -900 DEG C.
5. the high-ductility stabilized with yttrium oxide tetragonal zircite (3Y-TZP) that any described one kind of claim 2-4 is not influenced by sintering
The preparation method of material, which is characterized in that (3) the bulk preparation: the 3Y-TZP material is after 900 DEG C of heat treatment 1h
3Y-TZP nanometer powder is starting material, puts the powder into agate mortar and mills, and taking and being put into diameter in right amount is 18mm's
In stainless steel mould, molding disk is put into program-controlled high temperature furnace in 1350 DEG C -1600 by the compression moulding under 500MPa pressure
DEG C sintering 1.5-2.5h, temperature rate be 2 DEG C/min, be prepared into after being cooled to room temperature with a thickness of 2mm disk.
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| CN114394830A (en) * | 2021-12-28 | 2022-04-26 | 中红外激光研究院(江苏)有限公司 | Preparation method of high-strength zirconia ceramic |
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Effective date of registration: 20240613 Address after: 200941 Building 1, No. 7, Lane 577, Yuanhe Road, Baoshan District, Shanghai Patentee after: Shanghai Hengxin metal products manufacturing Co.,Ltd. Country or region after: China Address before: 621000, No. 59, Qinglong Avenue, Fucheng District, Sichuan, Mianyang Patentee before: Southwest University of Science and Technology Country or region before: China Patentee before: Leshan Jiajiang ecological environment monitoring station |