CN105777123A - Method for preparing transparent yttrium oxide ceramic component through two-step pressure sintering - Google Patents
Method for preparing transparent yttrium oxide ceramic component through two-step pressure sintering Download PDFInfo
- Publication number
- CN105777123A CN105777123A CN201610079474.9A CN201610079474A CN105777123A CN 105777123 A CN105777123 A CN 105777123A CN 201610079474 A CN201610079474 A CN 201610079474A CN 105777123 A CN105777123 A CN 105777123A
- Authority
- CN
- China
- Prior art keywords
- prepared
- transparent
- yttria ceramics
- ceramic powder
- transparent yttria
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000005245 sintering Methods 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 89
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title abstract description 14
- 239000011224 oxide ceramic Substances 0.000 title abstract 8
- 229910052574 oxide ceramic Inorganic materials 0.000 title abstract 8
- 239000000919 ceramic Substances 0.000 claims abstract description 134
- 239000000843 powder Substances 0.000 claims abstract description 73
- 238000000975 co-precipitation Methods 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000005498 polishing Methods 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 8
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 63
- 238000004448 titration Methods 0.000 claims description 30
- 238000001914 filtration Methods 0.000 claims description 21
- 238000012805 post-processing Methods 0.000 claims description 21
- 230000015572 biosynthetic process Effects 0.000 claims description 16
- 238000003786 synthesis reaction Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 230000032683 aging Effects 0.000 claims description 14
- 238000011010 flushing procedure Methods 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 14
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 7
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 206010016825 Flushing Diseases 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 7
- 239000001099 ammonium carbonate Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 16
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000002490 spark plasma sintering Methods 0.000 abstract 3
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 229910052727 yttrium Inorganic materials 0.000 abstract 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 13
- 229910010293 ceramic material Inorganic materials 0.000 description 10
- 238000005265 energy consumption Methods 0.000 description 8
- 230000010354 integration Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 238000005056 compaction Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 230000001629 suppression Effects 0.000 description 6
- 230000001737 promoting effect Effects 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011222 crystalline ceramic Substances 0.000 description 2
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
Classifications
-
- 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
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
- C04B35/505—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds based on yttrium oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/218—Yttrium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6565—Cooling rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
- C04B2235/662—Annealing after sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A method for preparing a transparent yttrium oxide ceramic component through two-step pressure sintering comprises the following steps that firstly, ceramic powder is synthesized, wherein high-purity superfine yttrium oxide nanometer ceramic powder is prepared with a reverse coprecipitation method; secondly, transparent yttrium oxide ceramic is sintered, wherein the transparent yttrium nanometer oxide ceramic is prepared with a two-step pressurized spark plasma sintering technology; thirdly, aftertreatment is carried out, wherein after spark plasma sintering, a sample is taken out for annealing and grinding polishing, and the final finished product, namely, the transparent yttrium oxide ceramic component, is obtained.According to the method for preparing the transparent yttrium oxide ceramic component through two-step pressure sintering, the nanometer yttrium oxide powder with a small particle size and uniform distribution is prepared in advance with the reverse coprecipitation method, and then the transparent yttrium oxide ceramic component good in compactness, uniform in particle size and good in performance is prepared with the two-step pressurized spark plasma sintering technology.The strength of the prepared transparent yttrium oxide ceramic component is higher than 400 MPa, and the transparence is higher than 60%.
Description
Technical field
The present invention relates to transparent yttria ceramics preparing technical field, particularly to a kind of method that transparent yttria ceramics parts are prepared in two step pressure sinterings.
Background technology
Transparent ceramic material is the Inorganic Non-metallic Materials of new generation that national security and national economy sustainable development are had great strategic significance by a class, the enforcement of country's Study on Long-team Strategy will be played the effect of actively promoting in following one period, therefore, carry out the Basic Science Problem research of crystalline ceramics and expand its application there is important profound significance.
In many transparent ceramic materials, yttrium oxide transparent ceramic receives significant attention with the performance of its excellence.Yittrium oxide is cubic system crystal, has optically isotropic character so that it has superior light transmission.Yttrium oxide transparent ceramic is made up in nineteen seventies of General Electric Apparatus Co.(U.S.A.) the earliest, its commercial " Yttralox " by name, its fusing point is up to 2400 DEG C, and in broad wavelength (0.3～8 μm) scope, particularly there is significantly high light transmittance in ultrared, therefore can serve as window pyrometer gate material, infrared through window material, high-temperature experiment apparatus material etc..Additionally, Y2O3Crystalline ceramics can be additionally used in microwave base plate, infrared emittance pipe, antenna house, missile IR window and ball cover etc..There is more significance, containing Nd2O3The Y added2O3Highly transparent pottery, laser technology can be used as the laser instrument solid material used at 1.064 mum wavelengths, yittrium oxide has low phonon energy and high heat conductance, and its thermal conductivity is higher than yttrium-aluminium-garnet (YAG), and accordingly act as high impulse laser instrument aspect more has prospect than YAG pottery.Additionally, due to the light transmittance of yittrium oxide and thermostability are above aluminium oxide ceramics, scholar is therefore had to expect to be applied to high-intensity gas discharge lamp field very early.As can be seen here, yttrium oxide transparent ceramic is the transparent ceramic material of a kind of structure set function integration, has wide application potential quality in many high-tech sectors.
The sintering processing of yttrium oxide transparent ceramic, is presently mainly vacuum (atmosphere) sintering and HIP sintering.These traditional sintering processings exist that heating rate is slow, efficiency is low, energy consumption is high, need pottery could realize densification at a higher temperature and there is the shortcomings such as easy to crack, defect is many for sintering.
Therefore, not enough for prior art, it is provided that a kind of two step pressure sinterings prepare the method for transparent yttria ceramics parts to overcome prior art deficiency very necessary.
Summary of the invention
A kind of method that it is an object of the invention to avoid the deficiencies in the prior art part and provide two step pressure sinterings to prepare transparent yttria ceramics parts, speed is fast, sintering temperature is low to have preparation, and prepared transparent yttria ceramics parts fine microstructure, compactness are good, function admirable.
The above-mentioned purpose of the present invention is realized by following technological means.
A kind of method providing two step pressure sinterings to prepare transparent yttria ceramics parts, comprises the steps:
(1) synthesis of ceramic powder: adopting reverse coprecipitation to prepare high pure and ultra-fine yittrium oxide nano ceramic powder, the purity of described high pure and ultra-fine yittrium oxide nano ceramic powder is more than 99.9%, and mean diameter is 80～200nm；
(2) sintering of transparent yttria ceramics: adopt the discharge plasma sintering process of two step pressurizations to prepare yittrium oxide nano transparent ceramic；
(3) post processing: after discharge plasma sintering, sample taking-up being annealed and carry out grinding and polishing obtains final finished product transparent yttria ceramics parts.
The mean diameter of above-mentioned high pure and ultra-fine yittrium oxide nano ceramic powder is 90nm.
The synthesis of above-mentioned steps (1) ceramic powder comprises the steps:
(1.1) weigh yittrium oxide raw material, dissolve with concentrated nitric acid, be configured to the yttrium nitrate solution that concentration is 0.2-0.8mol/L；
(1.2) yttrium nitrate solution is added drop-wise to concentration in the ammonium bicarbonate soln of 2～3mol/L by back titration method with the titration speed less than 5ml/min, the process of titration is stirred with magnetic stirrer simultaneously, making the pH value of solution be maintained at 9～11 by additionally dropping ammonia in titration process, reaction terminates rear ageing 1.0～2.0h；
(1.3) solution after (1.2) ageing is carried out sucking filtration, then carry out flushes sediment with ionized water and dehydrated alcohol respectively；
Repeating after flushing and carry out 4～5 sucking filtration, flushings, sucking filtration is placed 12～24h at the temperature of 80～90 DEG C after rinsing and is obtained precursor powder；
(1.4) precursor powder is sintered at 700～900 DEG C 2～3h, after sieving, obtain high pure and ultra-fine yittrium oxide nano ceramic powder.
In above-mentioned steps (1.2), in the process of titration, the stir speed (S.S.) of magnetic stirrer is 300～800rpm.
Above-mentioned steps (1.4) obtains high pure and ultra-fine yittrium oxide nano ceramic powder especially by the sieve that order number is 50～100 orders after sieving.
The discharge plasma sintering process of two step pressurizations of above-mentioned steps (2), its sintering schedule is: at the cold stage of room temperature～1000 DEG C, sinters when pressure is 8～12MPa；At the hot stage of 1000 DEG C～1450 DEG C, sinter when pressure is 95～110MPa.
Once entering, the discharge plasma sintering process of two step pressurizations of above-mentioned steps (2), its sintering schedule is: at the cold stage of room temperature～1000 DEG C, sinters when pressure is 10MPa；At the hot stage of 1000 DEG C～1450 DEG C, sinter when pressure is 100MPa.
Above-mentioned steps (2) two steps pressurization discharge plasma sintering process, its temperature increasing schedule particularly as follows:
It is 10～50 DEG C/min from the heating rate of room temperature～1000 DEG C, and is incubated 15～30min at 1000 DEG C；
It is 100～200 DEG C/min from the heating rates of 1000 DEG C～1450 DEG C, is incubated 5～10min at 1450 DEG C；
Release after 1450 DEG C of insulations terminate.
The annealing process of above-mentioned steps (3) post processing is specifically: be cooled to 800～1000 DEG C in air atmosphere, with the rate of temperature fall of 3～5 DEG C/min, and is incubated 5～12h at the temperature of 800～1000 DEG C.
The method that transparent yttria ceramics parts are prepared in the two step pressure sinterings of the present invention, comprise the steps: the synthesis of (1) ceramic powder: adopt reverse coprecipitation to prepare high pure and ultra-fine yittrium oxide nano ceramic powder, the purity of described high pure and ultra-fine yittrium oxide nano ceramic powder is more than 99.9%, and mean diameter is 80～200nm；(2) sintering of transparent yttria ceramics: adopt the discharge plasma sintering process of two step pressurizations to prepare yittrium oxide nano transparent ceramic；(3) post processing: after discharge plasma sintering, sample taking-up being annealed and carry out grinding and polishing obtains final finished product transparent yttria ceramics parts.The method of the present invention prepares that speed is fast, sintering temperature is low, and prepared transparent yttria ceramics parts fine microstructure, compactness are good, function admirable.
Detailed description of the invention
The invention will be further described with the following Examples.
Embodiment 1.
A kind of method that transparent yttria ceramics parts are prepared in two step pressure sinterings, comprises the steps:
(1) synthesis of ceramic powder: adopting reverse coprecipitation to prepare high pure and ultra-fine yittrium oxide nano ceramic powder, the purity of high pure and ultra-fine yittrium oxide nano ceramic powder is more than 99.9%, and mean diameter is 80～200nm, it is preferable that mean diameter is 90nm；
(2) sintering of transparent yttria ceramics: adopt the discharge plasma sintering process of two step pressurizations to prepare yittrium oxide nano transparent ceramic；
(3) post processing: after discharge plasma sintering, sample taking-up being annealed and carry out grinding and polishing obtains final finished product transparent yttria ceramics parts.
The two step pressure sinterings of the present invention prepare the method for transparent yttria ceramics parts by reverse coprecipitation method previously prepared go out particle diameter is less and the nano yttrium oxide powder that is evenly distributed, prepare that compactness is good again through the discharge plasma sintering process of two steps pressurizations, uniform particle sizes, function admirable transparent yttria ceramics parts.Prepared transparent yttria ceramics strength of parts is more than 400MPa, and transparency is more than 60%.
In addition the method for the present invention can sinter at programming rate faster, relatively low temperature, has programming rate fast, the feature that energy consumption is low.
Transparent yttria ceramics parts prepared by the method for the present invention can serve as structure-function integration ceramic material field.
Embodiment 2.
A kind of method that transparent yttria ceramics parts are prepared in two step pressure sinterings, carries out as follows.
(1) synthesis of ceramic powder: adopt reverse coprecipitation to prepare high pure and ultra-fine yittrium oxide nano ceramic powder, the purity of heretofore described high pure and ultra-fine yittrium oxide nano ceramic powder is more than 99.9%, mean diameter is 80～200nm, it is preferable that mean diameter is 90nm.
The synthesis of step (1) ceramic powder comprises the steps:
(1.1) weigh yittrium oxide raw material, dissolve with concentrated nitric acid, be configured to the yttrium nitrate solution that concentration is 0.2-0.8mol/L；
(1.2) yttrium nitrate solution is added drop-wise to concentration in the ammonium bicarbonate soln of 2～3mol/L by back titration method with the titration speed less than 5ml/min, the process of titration is stirred with the stir speed (S.S.) of 300～800rpm with magnetic stirrer simultaneously, making the pH value of solution be maintained at 9～11 by additionally dropping ammonia in titration process, reaction terminates rear ageing 1.0～2.0h；
(1.3) solution after (1.2) ageing is carried out sucking filtration, be then rinsed with ionized water and dehydrated alcohol respectively；
Repeating after flushing and carry out 4～5 sucking filtration, flushings, sucking filtration is placed 12～24h at the temperature of 80～90 DEG C after rinsing and is obtained precursor powder；
(1.4) precursor powder is sintered at 700～900 DEG C 2～3h, obtain high pure and ultra-fine yittrium oxide nano ceramic powder by after sieve that order number is 50～100 orders.
The yittrium oxide nano ceramic powder prepared by reverse coprecipitation method has the advantages that particle diameter is less and is evenly distributed, and the finished product prepared for follow-up sintering provides guarantee.
Prepare high pure and ultra-fine yittrium oxide nano-ceramic powder last, enter step (2) and be sintered.
(2) sintering of transparent yttria ceramics: adopt the discharge plasma sintering process of two step pressurizations to prepare yittrium oxide nano transparent ceramic.
The discharge plasma sintering process of two step pressurizations of step (2); its sintering schedule is: at the cold stage of room temperature～1000 DEG C; low pressure sintering is carried out when pressure is 8～12MPa; to release the high pressure suppression to grain sliding, promote that the sliding of crystal grain is thus eliminating open pore.At the hot stage of 1000 DEG C～1450 DEG C, carry out high-pressure sinter when pressure is 95～110MPa, it is achieved the high compaction of pottery.
Its temperature increasing schedule is particularly as follows: be 10～50 DEG C/min from the heating rate of room temperature～1000 DEG C, and is incubated 15～30min at 1000 DEG C；It is 100～200 DEG C/min from the heating rates of 1000 DEG C～1450 DEG C, is incubated 5～10min at 1450 DEG C；Release after 1450 DEG C of insulations terminate.
After sintering, enter step (3) post processing.
(3) post processing: after discharge plasma sintering, sample taking-up being annealed and carry out grinding and polishing obtains final finished product transparent yttria ceramics parts.
The annealing process of step (3) post processing is specifically: be cooled to 800～1000 DEG C in air atmosphere, with the rate of temperature fall of 3～5 DEG C/min, and is incubated 5～12h at the temperature of 800～1000 DEG C.
It is fast that the method for the present invention has programming rate, and the feature that energy consumption is low, the crystallite dimension of prepared transparent yttria ceramics parts is nanoscale, and particle size uniformity.Transparent yttria ceramics parts compactness is good, function admirable, and its intensity is more than 400MPa, and transparency, more than 60%, can be used as structure-function integration ceramic material field.
Embodiment 3.
A kind of method that transparent yttria ceramics parts are prepared in two step pressure sinterings; further feature is identical with embodiment 2; it is different in that: the discharge plasma sintering process of two step pressurizations of step (2); its sintering schedule is: at the cold stage of room temperature～1000 DEG C; sinter when pressure is 10MPa; to release the high pressure suppression to grain sliding, promote that the sliding of crystal grain is thus eliminating open pore；At the hot stage of 1000 DEG C～1450 DEG C, sinter when pressure is 100MPa, it is achieved the high compaction of pottery.
It is fast that the method for the present invention has programming rate, and the feature that energy consumption is low, the crystallite dimension of prepared transparent yttria ceramics parts is nanoscale, and particle size uniformity.Transparent yttria ceramics parts compactness is good, function admirable, and its intensity is more than 400MPa, and transparency, more than 60%, can be used as structure-function integration ceramic material field.
Embodiment 4.
A kind of method that transparent yttria ceramics parts are prepared in two step pressure sinterings, carries out as follows.
(1) synthesis of ceramic powder: adopting reverse coprecipitation to prepare high pure and ultra-fine yittrium oxide nano ceramic powder, the purity of heretofore described high pure and ultra-fine yittrium oxide nano ceramic powder is more than 99.9%, and mean diameter is 90 nanometers.
The synthesis of step (1) ceramic powder comprises the steps:
(1.1) weigh the yittrium oxide raw material that particle diameter is 80 nanometers, dissolve with concentrated nitric acid, be configured to the yttrium nitrate solution that concentration is 0.5mol/L；
(1.2) yttrium nitrate solution is added drop-wise to concentration in the ammonium bicarbonate soln of 2mol/L by back titration method with the titration speed of 2ml/min, the process of titration is stirred with the stir speed (S.S.) of 500rpm with magnetic stirrer simultaneously, making the pH value of solution be maintained at 10 by additionally dropping ammonia in titration process, reaction terminates rear ageing 1.0h；
(1.3) solution after (1.2) ageing is carried out sucking filtration, then with ionized water and dehydrated alcohol, precipitate is rinsed respectively；
Repeating after flushing and carry out 4～5 sucking filtration, flushings, sucking filtration is placed 24h at the temperature of 85 DEG C after rinsing and is obtained precursor powder；
(1.4) precursor powder is sintered at 800 DEG C 2h, obtain high pure and ultra-fine yittrium oxide nano ceramic powder by after sieve that order number is 80 orders.
The yittrium oxide nano ceramic powder prepared by reverse coprecipitation method has the advantages that particle diameter is less and is evenly distributed, and the finished product prepared for follow-up sintering provides guarantee.
Prepare high pure and ultra-fine yittrium oxide nano-ceramic powder last, enter step (2) and be sintered.
(2) sintering of transparent yttria ceramics: adopt the discharge plasma sintering process of two step pressurizations to prepare yittrium oxide nano transparent ceramic.
The discharge plasma sintering process of two step pressurizations of step (2); its sintering schedule is: at the cold stage of room temperature～1000 DEG C; carrying out low pressure sintering when pressure is 11MPa, to release the high pressure suppression to grain sliding, promoting that the sliding of crystal grain is thus eliminating open pore.At the hot stage of 1000 DEG C～1450 DEG C, carry out high-pressure sinter when pressure is 105MPa, it is achieved the high compaction of pottery.
Its temperature increasing schedule is particularly as follows: be 10 DEG C/min from the heating rate of room temperature～1000 DEG C, and is incubated 30min at 1000 DEG C；It is 100 DEG C/min from the heating rates of 1000 DEG C～1450 DEG C, is incubated 8min at 1450 DEG C；Release after 1450 DEG C of insulations terminate.
After sintering, enter step (3) post processing.
(3) post processing: after discharge plasma sintering, sample taking-up being annealed and carry out grinding and polishing obtains final finished product transparent yttria ceramics parts.
The annealing process of step (3) post processing is specifically: be cooled to 900 DEG C in air atmosphere, with the rate of temperature fall of 5 DEG C/min, and is incubated 5h at the temperature of 1000 DEG C.
It is fast that the method for the present invention has programming rate, and the feature that energy consumption is low, the crystallite dimension of prepared transparent yttria ceramics parts is nanoscale, and particle size uniformity.Transparent yttria ceramics parts compactness is good, function admirable, and its intensity is more than 400MPa, and transparency, more than 60%, can be used as structure-function integration ceramic material field.
Embodiment 5.
A kind of method that transparent yttria ceramics parts are prepared in two step pressure sinterings, carries out as follows.
(1) synthesis of ceramic powder: adopting reverse coprecipitation to prepare high pure and ultra-fine yittrium oxide nano ceramic powder, the purity of heretofore described high pure and ultra-fine yittrium oxide nano ceramic powder is more than 99.9%, and mean diameter is 88 nanometers.
The synthesis of step (1) ceramic powder comprises the steps:
(1.1) weigh yittrium oxide raw material, dissolve with concentrated nitric acid, be configured to the yttrium nitrate solution that concentration is 0.6mol/L；
(1.2) yttrium nitrate solution is added drop-wise to concentration in the ammonium bicarbonate soln of 3mol/L by back titration method with the titration speed less than 4ml/min, the process of titration is stirred with the stir speed (S.S.) of 700rpm with magnetic stirrer simultaneously, making the pH value of solution be maintained at 9.5 by additionally dropping ammonia in titration process, reaction terminates rear ageing 1.5h；
(1.3) solution after (1.2) ageing is carried out sucking filtration, be then rinsed with ionized water and dehydrated alcohol respectively；
Repeating after flushing and carry out 4～5 sucking filtration, flushings, sucking filtration is placed 12h at the temperature of 90 DEG C after rinsing and is obtained precursor powder；
(1.4) precursor powder is sintered at 900 DEG C 2h, obtain high pure and ultra-fine yittrium oxide nano ceramic powder by after sieve that order number is 50 orders.
The yittrium oxide nano ceramic powder prepared by reverse coprecipitation method has the advantages that particle diameter is less and is evenly distributed, and the finished product prepared for follow-up sintering provides guarantee.
Prepare high pure and ultra-fine yittrium oxide nano-ceramic powder last, enter step (2) and be sintered.
(2) sintering of transparent yttria ceramics: adopt the discharge plasma sintering process of two step pressurizations to prepare yittrium oxide nano transparent ceramic.
The discharge plasma sintering process of two step pressurizations of step (2); its sintering schedule is: at the cold stage of room temperature～1000 DEG C; carrying out low pressure sintering when pressure is 10.5MPa, to release the high pressure suppression to grain sliding, promoting that the sliding of crystal grain is thus eliminating open pore.At the hot stage of 1000 DEG C～1450 DEG C, carry out high-pressure sinter when pressure is 1050MPa, it is achieved the high compaction of pottery.
Its temperature increasing schedule is particularly as follows: be 50 DEG C/min from the heating rate of room temperature～1000 DEG C, and is incubated 30min at 1000 DEG C；It is 160 DEG C/min from the heating rates of 1000 DEG C～1450 DEG C, is incubated 10min at 1450 DEG C；Release after 1450 DEG C of insulations terminate.
After sintering, enter step (3) post processing.
(3) post processing: after discharge plasma sintering, sample taking-up being annealed and carry out grinding and polishing obtains final finished product transparent yttria ceramics parts.
The annealing process of step (3) post processing is specifically: be cooled to 980 DEG C in air atmosphere, with the rate of temperature fall of 5 DEG C/min, and is incubated 9h at the temperature of 800 DEG C.
It is fast that the method for the present invention has programming rate, and the feature that energy consumption is low, the crystallite dimension of prepared transparent yttria ceramics parts is nanoscale, and particle size uniformity.Transparent yttria ceramics parts compactness is good, function admirable, and its intensity is more than 400MPa, and transparency, more than 60%, can be used as structure-function integration ceramic material field.
Embodiment 6.
A kind of method that transparent yttria ceramics parts are prepared in two step pressure sinterings, carries out as follows.
(1) synthesis of ceramic powder: adopting reverse coprecipitation to prepare high pure and ultra-fine yittrium oxide nano ceramic powder, the purity of heretofore described high pure and ultra-fine yittrium oxide nano ceramic powder is more than 99.9%, and mean diameter is 100 microns.
The synthesis of step (1) ceramic powder comprises the steps:
(1.1) weigh yittrium oxide raw material, dissolve with concentrated nitric acid, be configured to the yttrium nitrate solution that concentration is 0.3mol/L；
(1.2) yttrium nitrate solution is added drop-wise to concentration in the ammonium bicarbonate soln of 2.5mol/L by back titration method with the titration speed of 4ml/min, the process of titration is stirred with the stir speed (S.S.) of 700rpm with magnetic stirrer simultaneously, making the pH value of solution be maintained at 9 by additionally dropping ammonia in titration process, reaction terminates rear ageing 1.8h；
(1.3) solution after (1.2) ageing is carried out sucking filtration, be then rinsed with ionized water and dehydrated alcohol respectively；
Repeating after flushing and carry out 3 sucking filtration, flushings, sucking filtration is placed 17h at the temperature of 90 DEG C after rinsing and is obtained precursor powder；
(1.4) precursor powder is sintered at 780 DEG C 2.6h, obtain high pure and ultra-fine yittrium oxide nano ceramic powder by after sieve that order number is 80 orders.
The yittrium oxide nano ceramic powder prepared by reverse coprecipitation method has the advantages that particle diameter is less and is evenly distributed, and the finished product prepared for follow-up sintering provides guarantee.
Prepare high pure and ultra-fine yittrium oxide nano-ceramic powder last, enter step (2) and be sintered.
(2) sintering of transparent yttria ceramics: adopt the discharge plasma sintering process of two step pressurizations to prepare yittrium oxide nano transparent ceramic.
The discharge plasma sintering process of two step pressurizations of step (2); its sintering schedule is: at the cold stage of room temperature～1000 DEG C; carrying out low pressure sintering when pressure is 11.5MPa, to release the high pressure suppression to grain sliding, promoting that the sliding of crystal grain is thus eliminating open pore.At the hot stage of 1000 DEG C～1450 DEG C, carry out high-pressure sinter when pressure is 100MPa, it is achieved the high compaction of pottery.
Its temperature increasing schedule is particularly as follows: be 40 DEG C/min from the heating rate of room temperature～1000 DEG C, and is incubated 20min at 1000 DEG C；It is 170 DEG C/min from the heating rates of 1000 DEG C～1450 DEG C, is incubated 6min at 1450 DEG C；Release after 1450 DEG C of insulations terminate.
After sintering, enter step (3) post processing.
(3) post processing: after discharge plasma sintering, sample taking-up being annealed and carry out grinding and polishing obtains final finished product transparent yttria ceramics parts.
The annealing process of step (3) post processing is specifically: be cooled to 900 DEG C in air atmosphere, with the rate of temperature fall of 4.5 DEG C/min, and is incubated 10h at the temperature of 1000 DEG C.
It is fast that the method for the present invention has programming rate, and the feature that energy consumption is low, the crystallite dimension of prepared transparent yttria ceramics parts is nanoscale, and particle size uniformity.Transparent yttria ceramics parts compactness is good, function admirable, and its intensity is more than 400MPa, and transparency, more than 60%, can be used as structure-function integration ceramic material field.
Embodiment 7.
A kind of method that transparent yttria ceramics parts are prepared in two step pressure sinterings, carries out as follows.
(1) synthesis of ceramic powder: adopting reverse coprecipitation to prepare high pure and ultra-fine yittrium oxide nano ceramic powder, the purity of heretofore described high pure and ultra-fine yittrium oxide nano ceramic powder is more than 99.9%, and mean diameter is 96 microns.
The synthesis of step (1) ceramic powder comprises the steps:
(1.1) weigh yittrium oxide raw material, dissolve with concentrated nitric acid, be configured to the yttrium nitrate solution that concentration is 0.7mol/L；
(1.2) yttrium nitrate solution is added drop-wise to concentration in the ammonium bicarbonate soln of 2.6mol/L by back titration method with the titration speed of 5ml/min, the process of titration is stirred with the stir speed (S.S.) of 400rpm with magnetic stirrer simultaneously, making the pH value of solution be maintained at 10.5 by additionally dropping ammonia in titration process, reaction terminates rear ageing 1.8h；
(1.3) solution after (1.2) ageing is carried out sucking filtration, be then rinsed with ionized water and dehydrated alcohol respectively；
Repeating after flushing and carry out 5 sucking filtration, flushings, sucking filtration is placed 19h at the temperature of 83 DEG C after rinsing and is obtained precursor powder；
(1.4) precursor powder is sintered at 820 DEG C 3h, obtain high pure and ultra-fine yittrium oxide nano ceramic powder by after sieve that order number is 80 orders.
The yittrium oxide nano ceramic powder prepared by reverse coprecipitation method has the advantages that particle diameter is less and is evenly distributed, and the finished product prepared for follow-up sintering provides guarantee.
Prepare high pure and ultra-fine yittrium oxide nano-ceramic powder last, enter step (2) and be sintered.
(2) sintering of transparent yttria ceramics: adopt the discharge plasma sintering process of two step pressurizations to prepare yittrium oxide nano transparent ceramic.
The discharge plasma sintering process of two step pressurizations of step (2); its sintering schedule is: at the cold stage of room temperature～1000 DEG C; carrying out low pressure sintering when pressure is 12MPa, to release the high pressure suppression to grain sliding, promoting that the sliding of crystal grain is thus eliminating open pore.At the hot stage of 1000 DEG C～1450 DEG C, carry out high-pressure sinter when pressure is 98MPa, it is achieved the high compaction of pottery.
Its temperature increasing schedule is particularly as follows: be 50 DEG C/min from the heating rate of room temperature～1000 DEG C, and is incubated 20min at 1000 DEG C；It is 100 DEG C/min from the heating rates of 1000 DEG C～1450 DEG C, is incubated 9min at 1450 DEG C；Release after 1450 DEG C of insulations terminate.
After sintering, enter step (3) post processing.
(3) post processing: after discharge plasma sintering, sample taking-up being annealed and carry out grinding and polishing obtains final finished product transparent yttria ceramics parts.
The annealing process of step (3) post processing is specifically: be cooled to 960 DEG C in air atmosphere, with the rate of temperature fall of 3～5 DEG C/min, and is incubated 10h at the temperature of 800～1000 DEG C.
It is fast that the method for the present invention has programming rate, and the feature that energy consumption is low, the crystallite dimension of prepared transparent yttria ceramics parts is nanoscale, and particle size uniformity.Transparent yttria ceramics parts compactness is good, function admirable, and its intensity is more than 400MPa, and transparency, more than 60%, can be used as structure-function integration ceramic material field.
Finally should be noted that; above example is only in order to illustrate technical scheme but not limiting the scope of the invention; although the present invention being explained in detail with reference to preferred embodiment; it will be understood by those within the art that; technical scheme can be modified or equivalent replacement, without deviating from the spirit and scope of technical solution of the present invention.
Claims (10)
1. the method that transparent yttria ceramics parts are prepared in a step pressure sintering, it is characterised in that comprise the steps:
(1) synthesis of ceramic powder: adopting reverse coprecipitation to prepare high pure and ultra-fine yittrium oxide nano ceramic powder, the purity of described high pure and ultra-fine yittrium oxide nano ceramic powder is more than 99.9%, and mean diameter is 80～200nm；
(2) sintering of transparent yttria ceramics: adopt the discharge plasma sintering process of two step pressurizations to prepare yittrium oxide nano transparent ceramic；
(3) post processing: after discharge plasma sintering, sample taking-up being annealed and carry out grinding and polishing obtains final finished product transparent yttria ceramics parts.
2. the method that transparent yttria ceramics parts are prepared in two step pressure sinterings according to claim 1, it is characterised in that the mean diameter of described high pure and ultra-fine yittrium oxide nano ceramic powder is 90nm.
3. the method that transparent yttria ceramics parts are prepared in two step pressure sinterings according to claim 1 and 2, it is characterised in that the synthesis of described step (1) ceramic powder comprises the steps:
(1.1) weigh yittrium oxide raw material, dissolve with concentrated nitric acid, be configured to the yttrium nitrate solution that concentration is 0.2～0.8mol/L；
(1.2) yttrium nitrate solution is added drop-wise to concentration in the ammonium bicarbonate soln of 2～3mol/L by back titration method with the titration speed less than 5ml/min, the process of titration is stirred with magnetic stirrer simultaneously, making the pH value of solution be maintained at 9～11 by additionally dropping ammonia in titration process, reaction terminates rear ageing 1.0～2.0h；
(1.3) solution after (1.2) ageing is carried out sucking filtration, then carry out flushes sediment with ionized water and dehydrated alcohol respectively；
Repeating after flushing and carry out 4～5 sucking filtration, flushings, sucking filtration is placed 12～24h at the temperature of 80～90 DEG C after rinsing and is obtained precursor powder；
(1.4) precursor powder is sintered at 700～900 DEG C 2～3h, after sieving, obtain high pure and ultra-fine yittrium oxide nano ceramic powder.
4. the method that transparent yttria ceramics parts are prepared in two step pressure sinterings according to claim 3, it is characterised in that in described step (1.2), in the process of titration, the stir speed (S.S.) of magnetic stirrer is 300～800rpm.
5. the method that transparent yttria ceramics parts are prepared in two step pressure sinterings according to claim 4, it is characterized in that, described step (1.4) obtains high pure and ultra-fine yittrium oxide nano ceramic powder especially by the sieve that order number is 50～100 orders after sieving.
6. the method that transparent yttria ceramics parts are prepared in two step pressure sinterings according to claim 3, it is characterised in that
The discharge plasma sintering process of two step pressurizations of described step (2), its sintering schedule is: at the cold stage of room temperature～1000 DEG C, sinters when pressure is 8～12MPa；At the hot stage of 1000 DEG C～1450 DEG C, sinter when pressure is 95～110MPa.
7. the method that transparent yttria ceramics parts are prepared in two step pressure sinterings according to claim 3, it is characterised in that
The discharge plasma sintering process of two step pressurizations of described step (2), its sintering schedule is: at the cold stage of room temperature～1000 DEG C, sinters when pressure is 10MPa；At the hot stage of 1000 DEG C～1450 DEG C, sinter when pressure is 100MPa.
8. the method that transparent yttria ceramics parts are prepared in two step pressure sinterings according to claim 7, it is characterised in that
Described step (2) two steps pressurization discharge plasma sintering process, its temperature increasing schedule particularly as follows:
It is 10～50 DEG C/min from the heating rate of room temperature～1000 DEG C, and is incubated 15～30min at 1000 DEG C；
It is 100～200 DEG C/min from the heating rates of 1000 DEG C～1450 DEG C, is incubated 5～10min at 1450 DEG C；
Release after 1450 DEG C of insulations terminate.
9. the method that transparent yttria ceramics parts are prepared in two step pressure sinterings according to claim 7, it is characterised in that
The annealing process of described step (3) post processing is specifically: be cooled to 800～1000 DEG C in air atmosphere, with the rate of temperature fall of 3～5 DEG C/min, and is incubated 5～12h at the temperature of 800～1000 DEG C.
10. the method that transparent yttria ceramics parts are prepared in two step pressure sinterings according to claim 1, it is characterized in that, the ceramic crystalline grain of prepared transparent yttria ceramics parts is of a size of nanoscale, the intensity of transparent yttria ceramics parts more than 400Mpa, transparency more than 60%.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610079474.9A CN105777123B (en) | 2016-02-04 | 2016-02-04 | A kind of method that the pressure sintering of two steps prepares transparent yttria ceramics component |
| PCT/CN2016/075448 WO2017133050A1 (en) | 2016-02-04 | 2016-03-03 | Two-step pressure sintering method for preparing transparent yttrium oxide ceramic part |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610079474.9A CN105777123B (en) | 2016-02-04 | 2016-02-04 | A kind of method that the pressure sintering of two steps prepares transparent yttria ceramics component |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105777123A true CN105777123A (en) | 2016-07-20 |
| CN105777123B CN105777123B (en) | 2018-08-21 |
Family
ID=56403287
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610079474.9A Expired - Fee Related CN105777123B (en) | 2016-02-04 | 2016-02-04 | A kind of method that the pressure sintering of two steps prepares transparent yttria ceramics component |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN105777123B (en) |
| WO (1) | WO2017133050A1 (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106380196A (en) * | 2016-08-29 | 2017-02-08 | 彭展忠 | Molding technology of ceramic cutting tool |
| CN106396673A (en) * | 2016-08-29 | 2017-02-15 | 彭展忠 | Processing technology of ceramic cutter |
| CN106396674A (en) * | 2016-08-29 | 2017-02-15 | 彭展忠 | Production method of high-toughness ceramic cutter |
| CN106396672A (en) * | 2016-08-29 | 2017-02-15 | 彭展忠 | Production method of ceramic cutte |
| CN106588015A (en) * | 2016-12-23 | 2017-04-26 | 东华大学 | Method for preparing yttrium oxide ceramic based on mesoporous yttrium oxide |
| CN107673390A (en) * | 2017-10-10 | 2018-02-09 | 厦门大学 | A kind of preparation method of exquisite spherical nano yttrium oxide |
| CN108546097A (en) * | 2018-07-03 | 2018-09-18 | 洛阳欣珑陶瓷有限公司 | Ice porcelain and its preparation process |
| CN109467434A (en) * | 2018-12-27 | 2019-03-15 | 东北大学 | A kind of high-fracture toughness high-heat resistance shock resistant Yttrium oxide material and preparation method thereof |
| CN115677341A (en) * | 2021-07-28 | 2023-02-03 | 中国科学院上海硅酸盐研究所 | Bismuth-layered ferroelectric ceramic with high transparency and preparation method thereof |
| CN116675536A (en) * | 2023-05-11 | 2023-09-01 | 武汉科技大学 | Yttria ceramic crucible for smelting titanium alloy and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174645B (en) * | 2020-09-27 | 2022-05-31 | 中国科学院上海光学精密机械研究所 | Method for preparing compact nano-crystalline ceramic |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698601A (en) * | 2009-11-04 | 2010-04-28 | 中国科学院上海硅酸盐研究所 | Sintering method of yttrium oxide base transparent ceramic |
| CN102020470A (en) * | 2009-09-17 | 2011-04-20 | 中国科学院上海硅酸盐研究所 | Preparation method of transparent yttria ceramics with high optical quality |
| CN102190499A (en) * | 2010-03-18 | 2011-09-21 | 中国科学院福建物质结构研究所 | Preparation method of transparent yttria ceramic |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224974A (en) * | 2007-08-24 | 2008-07-23 | 中国科学院上海硅酸盐研究所 | Yttrium-aluminium series small crystal transparent ceramic material and preparation method |
| CN101269964A (en) * | 2008-04-29 | 2008-09-24 | 烁光特晶科技有限公司 | Method for preparing yttrium oxide transparent ceramic |
| CN104529449A (en) * | 2014-12-18 | 2015-04-22 | 徐州市江苏师范大学激光科技有限公司 | Method for preparing yttrium oxide-based transparent ceramic employing two-step sintering method |
-
2016
- 2016-02-04 CN CN201610079474.9A patent/CN105777123B/en not_active Expired - Fee Related
- 2016-03-03 WO PCT/CN2016/075448 patent/WO2017133050A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020470A (en) * | 2009-09-17 | 2011-04-20 | 中国科学院上海硅酸盐研究所 | Preparation method of transparent yttria ceramics with high optical quality |
| CN101698601A (en) * | 2009-11-04 | 2010-04-28 | 中国科学院上海硅酸盐研究所 | Sintering method of yttrium oxide base transparent ceramic |
| CN102190499A (en) * | 2010-03-18 | 2011-09-21 | 中国科学院福建物质结构研究所 | Preparation method of transparent yttria ceramic |
Non-Patent Citations (1)
| Title |
|---|
| 周国红 等: "大尺寸透明氧化钇陶瓷的制备", 《中国空间科学学会空间材料专业委员会2009学术交流会》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106380196A (en) * | 2016-08-29 | 2017-02-08 | 彭展忠 | Molding technology of ceramic cutting tool |
| CN106396673A (en) * | 2016-08-29 | 2017-02-15 | 彭展忠 | Processing technology of ceramic cutter |
| CN106396674A (en) * | 2016-08-29 | 2017-02-15 | 彭展忠 | Production method of high-toughness ceramic cutter |
| CN106396672A (en) * | 2016-08-29 | 2017-02-15 | 彭展忠 | Production method of ceramic cutte |
| CN106588015A (en) * | 2016-12-23 | 2017-04-26 | 东华大学 | Method for preparing yttrium oxide ceramic based on mesoporous yttrium oxide |
| CN107673390A (en) * | 2017-10-10 | 2018-02-09 | 厦门大学 | A kind of preparation method of exquisite spherical nano yttrium oxide |
| CN107673390B (en) * | 2017-10-10 | 2019-04-26 | 厦门大学 | A kind of preparation method of exquisite spherical nano yttrium oxide |
| CN108546097A (en) * | 2018-07-03 | 2018-09-18 | 洛阳欣珑陶瓷有限公司 | Ice porcelain and its preparation process |
| CN109467434A (en) * | 2018-12-27 | 2019-03-15 | 东北大学 | A kind of high-fracture toughness high-heat resistance shock resistant Yttrium oxide material and preparation method thereof |
| CN115677341A (en) * | 2021-07-28 | 2023-02-03 | 中国科学院上海硅酸盐研究所 | Bismuth-layered ferroelectric ceramic with high transparency and preparation method thereof |
| CN116675536A (en) * | 2023-05-11 | 2023-09-01 | 武汉科技大学 | Yttria ceramic crucible for smelting titanium alloy and preparation method thereof |
| CN116675536B (en) * | 2023-05-11 | 2024-04-30 | 武汉科技大学 | Yttria ceramic crucible for smelting titanium alloy and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105777123B (en) | 2018-08-21 |
| WO2017133050A1 (en) | 2017-08-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105777123A (en) | Method for preparing transparent yttrium oxide ceramic component through two-step pressure sintering | |
| Xu et al. | Synthesis of monodispersed spherical yttrium aluminum garnet (YAG) powders by a homogeneous precipitation method | |
| Jin et al. | ZrO2-doped Y2O3 transparent ceramics via slip casting and vacuum sintering | |
| Ikesue et al. | Synthesis of Nd3+, Cr3+‐codoped YAG ceramics for high‐efficiency solid‐state lasers | |
| Li et al. | Co-precipitation synthesis and two-step sintering of YAG powders for transparent ceramics | |
| Ghaderi et al. | Spark plasma sintering of transparent Y2O3 ceramic using hydrothermal synthesized nanopowders | |
| Razavi et al. | Effect of sintering temperature on microstructural and optical properties of transparent yttria ceramics fabricated by spark plasma sintering | |
| Wang et al. | Microwave synthesis of homogeneous YAG nanopowder leading to a transparent ceramic | |
| CN105601277A (en) | Preparation method of yttrium oxide-based transparent ceramic | |
| Liu et al. | Fabrication of fine-grained undoped Y2O3 transparent ceramic using nitrate pyrogenation synthesized nanopowders | |
| Li et al. | Post-treatment of nanopowders-derived Nd: YAG transparent ceramics by hot isostatic pressing | |
| Liu et al. | Fabrication and characterizations of 8.7 mol% Y2O3-ZrO2 transparent ceramics using co-precipitated nanopowders | |
| Jing et al. | High efficiency synthesis of Nd: YAG powder by a spray co-precipitation method for transparent ceramics | |
| Huang et al. | Synthesis of mono-dispersed spherical Nd: Y2O3 powder for transparent ceramics | |
| Huang et al. | Fabrication of Y2O3 transparent ceramics by hot isostatic pressing from precipitated nanopowders | |
| CN104387081A (en) | Low-temperature preparation method of transparent aluminum oxynitride (AlON) ceramic | |
| Huang et al. | An effective strategy for preparing transparent ceramics using nanorod powders based on pressure-assisted particle fracture and rearrangement | |
| Zhao et al. | Vacuum sintering of highly transparent La1. 28Yb1. 28Zr2O7. 84 ceramic using nanosized raw powders | |
| US20140151913A1 (en) | Cost effective y2o3 synthesis and related functional nanocomposites | |
| Li et al. | Comparison of commercial and synthesized CaF2 powders for preparing transparent ceramics | |
| Kokuoz et al. | Er‐Doped Y2O3 Nanoparticles: A Comparison of Different Synthesis Methods | |
| CN103265286B (en) | Method for low-temperature preparation of Y2O3 and MgO codoped ZrO2 transparent ceramic through microwave sintering | |
| CN112174645B (en) | Method for preparing compact nano-crystalline ceramic | |
| CN108046794B (en) | Method for preparing yttrium titanate transparent ceramic by using coprecipitation method synthetic powder | |
| CN101891217A (en) | Method for preparing high-purity rare earth boride 6 (REB6) nano-powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180821 |