CN106799783A - A kind of isostatic cool pressing method and the preparation method of optical ceramics suitable for optical ceramics - Google Patents
A kind of isostatic cool pressing method and the preparation method of optical ceramics suitable for optical ceramics Download PDFInfo
- Publication number
- CN106799783A CN106799783A CN201710073673.3A CN201710073673A CN106799783A CN 106799783 A CN106799783 A CN 106799783A CN 201710073673 A CN201710073673 A CN 201710073673A CN 106799783 A CN106799783 A CN 106799783A
- Authority
- CN
- China
- Prior art keywords
- isostatic cool
- embryo
- cylinder
- cool pressing
- ceramics
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 110
- 238000003825 pressing Methods 0.000 title claims abstract description 90
- 230000003287 optical effect Effects 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 210000001161 mammalian embryo Anatomy 0.000 claims abstract description 102
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000003755 preservative agent Substances 0.000 claims abstract description 20
- 230000002335 preservative effect Effects 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims description 29
- 238000000498 ball milling Methods 0.000 claims description 24
- 238000007873 sieving Methods 0.000 claims description 14
- 239000002223 garnet Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 7
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- PSNPEOOEWZZFPJ-UHFFFAOYSA-N alumane;yttrium Chemical compound [AlH3].[Y] PSNPEOOEWZZFPJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 210000002257 embryonic structure Anatomy 0.000 claims description 3
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 9
- 230000007547 defect Effects 0.000 abstract description 6
- 238000005498 polishing Methods 0.000 abstract description 6
- 238000002834 transmittance Methods 0.000 abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 22
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 18
- 238000001354 calcination Methods 0.000 description 12
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 10
- 229910052721 tungsten Inorganic materials 0.000 description 10
- 239000010937 tungsten Substances 0.000 description 10
- 238000005303 weighing Methods 0.000 description 8
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 230000006378 damage Effects 0.000 description 5
- 230000013020 embryo development Effects 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 3
- 241000219991 Lythraceae Species 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 235000014360 Punica granatum Nutrition 0.000 description 2
- -1 Yttrium-erbium-aluminum Chemical compound 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000037237 body shape Effects 0.000 description 2
- 239000011222 crystalline ceramic Substances 0.000 description 2
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- MVLMQGYYLCWMFP-UHFFFAOYSA-N neodymium yttrium Chemical compound [Y].[Nd] MVLMQGYYLCWMFP-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/003—Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
-
- 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
- C04B35/44—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 aluminates
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials For Medical Uses (AREA)
- Prostheses (AREA)
Abstract
The invention provides a kind of isostatic cool pressing method and the preparation method of optical ceramics suitable for optical ceramics, isostatic cool pressing method is comprised the following steps：A) some optical ceramics cylindrical shapes element embryo after will be dry-pressing formed is stacked between a cylinder, and each two cylindrical shape element embryo and is separated with circular pan paper；B) cylinder for being stacked into step a) wraps up at least 2 layers with preservative film；C) cylinder that step b) is wrapped is put into vacuum bag and is vacuumized, then isostatic cool pressing, the optical ceramics element embryo after obtaining isostatic cool pressing through release.Using the method for the new isostatic cool pressing of the present invention, edge can be prepared and be damaged less ceramic idiosome, and then prepare the potsherd with high transmittance.It is demonstrated experimentally that the Nd that the embodiment of the present invention is sintered out using new isostatic cool pressing technology：YAG laser ceramics edge defects are greatly reduced, and transmitance is up to 81% after polishing.
Description
Technical field
The present invention relates to optical ceramics technical field, more particularly to a kind of isostatic cool pressing method suitable for optical ceramics and
The preparation method of optical ceramics.
Background technology
Optical ceramics, because type of feed, preparation method difference are different with products obtained therefrom kind, can have resistance to height also known as crystalline ceramics
The excellent specific property such as warm, corrosion-resistant, resistance to erosion, high intensity, they are in laser technology, space technology, electricity, optics, chemical industry, metallurgy
Etc. aspect be widely used.At present, conventional optical ceramics has aluminum oxide, magnesia, yttria (Y2O3), calcirm-fluoride,
Beryllium oxide, gadolinium sesquioxide (Gd2O3), calcium oxide, thorium oxide (ThO2) and PLZT ceramics (PLZT) etc..
Wherein, Nd：YAG laser ceramicses in detection, energy-conservation, medical science, are swashed as a kind of laser working medium of laser
The aspects such as light, exploration have huge international market, and with wide application prospect.Yttrium-aluminium-garnet (Y3Al5O12, yttrium
Aluminum garnet, YAG) there is excellent optical property, it is widely used in laser matrix material.1989,
M.Sekita et al. is prepared on the basis of YAG crystalline ceramics in G.Dewith et al., using homogeneous co-precipitation process, is made with urea
For precipitating reagent prepares Nd3+:YAG precursor powders, through molded and vacuum-sintering of cooling down, obtain transparent Nd3+:YAG ceramics materials
Material, but there is no laser output.For many years, Nd:YAG obtains sustainable development, and performance is improved constantly.And prepared with solid phase method and swashed
The features such as light ceramic is due to low cost, process is simple is favored by people.
Specifically, solid reaction process need to be by well mixed powder, by dry-pressing formed and isostatic cool pressing method, pressure
Into the cylindrical idiosome of high-compactness.In prepared by general laser ceramics, need to be by dry-pressing formed idiosome one during isostatic cool pressing
Each and every one is fitted into vacuum bag.But, because vacuum bag does not possess improved flexibility, easily in isostatic cool pressing or when vacuumizing pair
The corner angle of cylindrical idiosome produce destruction, cause the transmitance of potsherd periphery to decline due to the presence of these defects.Furthermore
In usual cold isostatic pressing process, because vacuum bag has certain hardness, when vacuumizing, still easily deposited in vacuum bag and plain embryo
In gap, so in isostatic cool pressing, stress is easily uneven, causes the consistency of ceramic partially than relatively low, and defect is more, pottery
The transmitance reduction of porcelain.
The content of the invention
In view of this, the application provides a kind of isostatic cool pressing method and the preparation side of optical ceramics suitable for optical ceramics
Method, using the method for the new isostatic cool pressing of the present invention, can prepare edge and be damaged less ceramic idiosome, and then preparation is provided
There is the potsherd of high transmittance.
The present invention provides a kind of isostatic cool pressing method suitable for optical ceramics, comprises the following steps：
A) some optical ceramics cylindrical shapes element embryo after will be dry-pressing formed is stacked into a cylinder, and each two is justified
Separated with circular pan paper between bar shape element embryo；
B) cylinder for being stacked into step a) wraps up at least 2 layers with preservative film；
C) cylinder that step b) is wrapped is put into vacuum bag and is vacuumized, then isostatic cool pressing, obtain cold through release
Optical ceramics element embryo after isostatic pressed.
Preferably, the number of some optical ceramics cylindrical shape element embryos is 10~20；Each cylindrical shape element embryo
Height be 10mm~30mm.
Preferably, the circular pan paper with diameter greater than the diameter equal to cylinder.Wherein, the diameter of circular pan paper
Should try one's best identical with cylinder diameter, if preventing follow-up preservative film used from pressing close to ceramics well compared with conference, if compared with
It is small to cause upper and lower idiosome marginal portion directly contact, it is impossible to reach the effect for completely cutting off upper and lower powder.
Preferably, the cylinder that be stacked into for step a) by the step b) wraps up 3~4 layers with preservative film.
Preferably, the pressure of the step c) isostatic cool pressings is 200MPa~250MPa, and the time is 3 minutes~5 minutes.
Preferably, the speed of the step c) releases is 20MPa/min~30MPa/min.
Preferably, it is described it is dry-pressing formed after some optical ceramics cylindrical shapes element embryo by following methods obtain：
Precursor powder is sequentially passed through into ball milling, sieving and is calcined, it is then dry-pressing formed, obtain some optical ceramics cylinders
Body shape element embryo.
Preferably, the dry-pressing formed pressure is 20MPa~50MPa, and the time is 3 minutes~5 minutes.
Preferably, the optical ceramics cylindrical shape element embryo is to generally use the optics that solid phase method is prepared and needs transmitance
Ceramics, include but is not limited to mix rare-earth yttrium-aluminium garnet element embryo, GaF2Plain embryo or Lu2O3This is several for plain embryo.
The present invention also provides a kind of preparation method of optical ceramics, comprises the following steps：
A) some optical ceramics cylindrical shapes element embryo after will be dry-pressing formed is stacked into a cylinder, and each two is justified
Separated with circular pan paper between bar shape element embryo；
B) cylinder for being stacked into step a) wraps up at least 2 layers with preservative film；
C) cylinder that step b) is wrapped is put into vacuum bag and is vacuumized, then isostatic cool pressing, obtain cold through release
Optical ceramics element embryo after isostatic pressed；
D) by after step c) isostatic cool pressings optical ceramics element embryo calcined successively, vacuum-sintering, annealing and polish, obtain
To optical ceramics.
Compared with prior art, the small column voxel embryo after the present invention will be dry-pressing formed is stacked into one greatly one by one
Cylinder, and separate each two small column voxel embryo, one entirety of plain embryogenesis for so stacking, energy with circular pan paper
The plain embryo marginal position of center section is set to be protected well.Bag of the present invention also with preservative film by the plain embryo of heap poststack tightly
Firmly, so soft preservative film can not only make one entirety of plain embryogenesis of stacking, and also may be used in follow-up isostatic cool pressing
As buffer strip, it is to avoid vacuum bag produces destruction to plain embryo, can also make each position uniform force of plain embryo.It is demonstrated experimentally that this
The Nd that inventive embodiments are sintered out using new isostatic cool pressing technology:YAG laser ceramics edge defects are greatly reduced, polishing
Transmitance is up to 81% afterwards.Therefore, using the method for the new isostatic cool pressing of the present invention, edge can be prepared and is damaged less pottery
Porcelain idiosome, and then prepare the potsherd with high transmittance.
Brief description of the drawings
Fig. 1 is the schematic diagram of the dry-pressing formed plain embryo stacking of the embodiment of the present invention；
Fig. 2 is the impaired analysis chart of plain embryo after prior art and embodiment of the present invention isostatic cool pressing；
Fig. 3 is the photo in kind of the gained laser ceramics of the embodiment of the present invention 1；
Fig. 4 is the photo in kind of the gained laser ceramics of comparative example of the present invention 1；
Fig. 5 is the photo in kind of the gained laser ceramics of the embodiment of the present invention 2；
Fig. 6 is the photo in kind of the gained laser ceramics of comparative example of the present invention 2.
Specific embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
The invention provides a kind of isostatic cool pressing method suitable for optical ceramics, comprise the following steps：
A) some optical ceramics cylindrical shapes element embryo after will be dry-pressing formed is stacked into a cylinder, and each two is justified
Separated with circular pan paper between bar shape element embryo；
B) cylinder for being stacked into step a) wraps up at least 2 layers with preservative film；
C) cylinder that step b) is wrapped is put into vacuum bag and is vacuumized, then isostatic cool pressing, obtain cold through release
Optical ceramics element embryo after isostatic pressed.
Invention broadly provides a kind of method of new isostatic cool pressing, with the method can prepare edge be damaged it is less
Ceramic idiosome, and then prepare the potsherd with high transmittance.
The embodiment of the present invention prepare first it is dry-pressing formed after optical ceramics cylindrical shape element embryo, the optical ceramics cylinder
Body shape element embryo can be to mix rare-earth yttrium-aluminium garnet element embryo, such as mix the yttrium-aluminium-garnet element embryo of Yb, Er, Nd, Ce, or
GaF2Plain embryo or Lu2O3The optical ceramics such as plain embryo element embryo.In some embodiments of the invention, the optical ceramics cylindrical shape
Plain embryo is neodymium-doped yttrium-aluminum garnet element embryo or mixes bait yttrium-aluminium-garnet element embryo；Rare earth volume is usually 0.5wt%~5wt%.
In a preferred embodiment of the invention, it is described it is dry-pressing formed after some optical ceramics cylindrical shapes element embryo according to
Lower method is obtained：Precursor powder is sequentially passed through into ball milling, sieving and is calcined, it is then dry-pressing formed, obtain some optical ceramics
Cylindrical shape element embryo.
Wherein, the ball milling, sieving and calcining etc. are all technological means well-known to those skilled in the art, and the present invention does not have
Have specifically limited.The dry-pressing formed pressure is preferably 20MPa~50MPa；Time is preferably 3 minutes~5 minutes.
The method that some embodiments of the invention prepare the dry-pressing formed plain embryo of neodymium-doped yttrium-aluminum garnet is comprised the following steps that：By phase
The Y that should be measured2O3、Al2O3、Nd2O3After mixing, a certain amount of teos is added as additive, alcohol is used as ball milling agent；With corresponding amount
High purity aluminium oxide ball as ball milling ball, ball milling 960min~980min under the rotating speed of 240rpm~250rpm.After ball milling, can
24h is dried in 80 DEG C, then ball and powder is separated with the screen cloth of 200 mesh and the sieving to powder.Powder after sieving is put
Enter and calcine 3h~5h in Muffle furnace at 800 DEG C~1000 DEG C.By the preferably pressurize under 20MPa within the compressor of the powder after calcining
3 minutes, can the dry-pressing formed neodymium-doped yttrium-aluminum garnet element embryo into 16mm × 16mm.
Obtain it is dry-pressing formed after some optical ceramics small cylinder shapes element embryo after, the embodiment of the present invention by they one connect
One is stacked into a big cylinder, and is separated with circle pan paper between each two cylindrical shape element embryo.
As shown in figure 1, Fig. 1 is the schematic diagram of the dry-pressing formed plain embryo stacking of the embodiment of the present invention.The present invention implements to do
The small column voxel embryo of the 16mm × 16mm after molded is stacked into a big cylinder one by one, and each two piece is used
The weighing scraps of paper that the circle of one Xiao Zhang 16mm × 16mm is soft separate, and one entirety of plain embryogenesis of stacking makes the element of center section
Embryo marginal position is protected well.
In an embodiment of the present invention, the number of some optical ceramics cylindrical shape element embryos can be 10~20.Root
Different according to die size, the height of each cylindrical shape element embryo can be 10mm~30mm, such as plain embryo size be 16mm × 16mm or
10mm×10mm.In the present invention, the circular pan paper is not easy to make ceramics be stained with impurity, using weighing commonly used in the art
The scraps of paper.The diameter of the circular pan paper is preferably greater than or equal to the diameter of cylinder, but conference causes follow-up parcel not excessively
Tightly.
The above-mentioned cylinder being stacked into is wrapped up at least 2 layers, preferably wraps up 3~4 layers by the embodiment of the present invention with preservative film.Its
In, the preservative film is weak, clean, can wrap up tight, using membrane product well known to those skilled in the art.
In some embodiments of the invention, the neodymium-doped yttrium-aluminum garnet of heap poststack is swashed with soft, clean preservative film
Light ceramic element embryo is closely encased, and that is tried one's best during parcel discharges the air in sack, repeats 3~4 times.In the present invention, it is soft
Soft preservative film can not only make one entirety of plain embryogenesis of stacking, and in isostatic cool pressing can also as buffer strip,
Vacuum bag is avoided to produce destruction to plain embryo.
The plain embryo cylinder that the embodiment of the present invention is wrapped is vacuumized in being put into vacuum bag, then will exhaust the sack after vacuum
Being put into cold isostatic press carries out isostatic cool pressing, through release, obtains the element embryo of the optical ceramics after isostatic cool pressing.
In the present invention, described being put into vacuum bag vacuumizes the technological means being well known to those skilled in the art.Institute
State the pressure preferably 200MPa~250MPa of isostatic cool pressing；Time is preferably 3 minutes~5 minutes.After vacuumizing end, this hair
Bright use cold isostatic press, isostatic cool pressing 3 minutes preferably under the pressure of 200MPa.During release, the embodiment of the present invention can allow cold
Pressure in isostatic pressing machine slowly declines according to certain speed；The speed of release is preferably 20MPa/min~30MPa/min.
After release, the embodiment of the present invention takes out the plain embryo in vacuum bag, that is, obtain the optical ceramics element embryo of high-compactness such as
Nd:YAG laser ceramicses element embryo.Fig. 2 is the impaired analysis chart of plain embryo after prior art and embodiment of the present invention isostatic cool pressing, this hair
Plain embryo cylinder is put into the mode of vacuum bag reference can be made to Fig. 2 in bright embodiment.Figure it is seen that prior art is easily to circle
The corner angle of cylindricality idiosome produce destruction, and idiosome has corner angle vulnerable zone；And the embodiment of the present application is using soft preservative film parcel heap
The plain embryo of poststack, can not only make one entirety of plain embryogenesis of stacking, and buffer strip can also be played in isostatic cool pressing
Effect, it is to avoid the plain embryo of vacuum bag destruction, so that the ceramic idiosome edge prepared is damaged less, performance is good.
Present invention also offers a kind of preparation method of optical ceramics, comprise the following steps：
A) some optical ceramics cylindrical shapes element embryo after will be dry-pressing formed is stacked into a cylinder, and each two is justified
Separated with circular pan paper between bar shape element embryo；
B) cylinder for being stacked into step a) wraps up at least 2 layers with preservative film；
C) cylinder that step b) is wrapped is put into vacuum bag and is vacuumized, then isostatic cool pressing, obtain cold through release
Optical ceramics element embryo after isostatic pressed；
D) by after step c) isostatic cool pressings optical ceramics element embryo calcined successively, vacuum-sintering, annealing and polish, obtain
To optical ceramics.
The present invention obtains the particular content of the preparation process of the optical ceramics element embryo after isostatic cool pressing as it was previously stated, herein not
Repeat again.
Pressure release is sampled, and after obtaining the element embryo of the optical ceramics after isostatic cool pressing, the embodiment of the present invention is put it into Muffle furnace
Calcined.The temperature of the calcining is preferably 800~900 DEG C；It is preferred that calcining 3h~4h.Then, the embodiment of the present invention is by element
Embryo is put into vacuum tungsten coil furnace, carries out vacuum-sintering, treats that tungsten coil furnace is cooled to room temperature, can obtain ceramics.
In some currently preferred embodiments of the present invention, the vacuum-sintering is specially：It is raised to the speed of 5~10 DEG C/min
1000 DEG C, then it is raised to 1700 DEG C~1800 DEG C with the speed of 1~2 DEG C/min.Insulation 10 hours~12 hours, then with 5~10
DEG C/speed of min cools to 1000 DEG C, obtains ceramics.
The embodiment of the present invention is annealed and is polished to vacuum-sintering gained ceramics, obtains optical ceramics finished product.Wherein, institute
The technology contents that annealing and polishing are well known to the skilled person are stated, the present invention is not particularly limited.Finally, the present invention
Embodiment can obtain Nd3+The YAG laser ceramicses of doping, Er3+The optical ceramics such as the YAG laser ceramicses of doping.
Using method of testings such as the conventional ceramic transmitances in this area, performance test is carried out to potsherd after polishing.Experiment
Prove, the Nd that the embodiment of the present invention is sintered out using new isostatic cool pressing technology:YAG laser ceramics edge defects greatly subtract
Few, up to 81%, potsherd transmitance is high, beneficial to application for transmitance after polishing.
For a further understanding of the application, with reference to embodiment the application is provided suitable for the cold etc. of optical ceramics
The preparation method of static pressure method and optical ceramics is specifically described.
Embodiment 1
The method and step that the present invention prepares Nd-doped Yttrium Aluminum Garnet Ceramics is as follows：
(1) according to mol ratio Y：Al=3:5、Nd:Y=1:99, the accurate Y for weighing respective amount2O3、Al2O3、Nd2O3Put
Enter in ball grinder, add a certain amount of teos as additive, alcohol is used as ball milling agent.Add the high purity aluminium oxide ball of corresponding amount
As ball milling ball, it is put into ball mill under the rotating speed of 240rpm, ball milling 960min.Wherein, teos is according to total powder quality
0.5% weighs, and alumina balls then press powder：Alcohol：Sphere volume ratio is 1：4：4 are added.
(2) ball grinder after ball milling is put into and dries 24h in drying box in 80 DEG C, then with the screen cloth of 200 mesh to ball and
Powder is separated and the sieving to powder.
(3) powder after sieving is put into Muffle furnace and calcines 3h at 800 DEG C.
(4) it is dry-pressing formed into 16mm × 16mm's by the powder after calcining within the compressor in pressurize under 20MPa 3 minutes
Neodymium-doped yttrium-aluminum garnet element embryo.
(5) the small column voxel embryo (totally 10) of the 16mm × 16mm after will be dry-pressing formed is stacked into one one by one
Cylinder, and each two piece greatly is separated with the soft weighing scraps of paper of the circle of an Xiao Zhang 16mm × 16mm.
(6) with soft, clean preservative film (the conventional preservative film of the food of net purchase) by the neodymium doped yttrium aluminum pomegranate of heap poststack
Stone laser ceramics element embryo is closely encased, and that is tried one's best during parcel discharges the air in sack, is repeated 4 times.
(7) after the plain embryo that will be wrapped is put into and is vacuumized in vacuum bag, it is put into cold etc. in 200MPa in cold isostatic press
Static pressure 3 minutes, release sampling.
(8) the plain embryo of gained after isostatic cool pressing is put into Muffle furnace and calcines 3h at 800 DEG C.
(9) by calcining after plain embryo be put into vacuum tungsten coil furnace, be raised to 1000 DEG C with the speed of 10 DEG C/min, then with 1.5
DEG C/speed of min is raised to 1750 DEG C, is incubated 10 hours, then cools to 1000 DEG C with the speed of 10 DEG C/min, treats that tungsten coil furnace is cold
But to acquisition ceramics after room temperature.
(10) ceramics annealed, polished, obtained Nd3+YAG laser ceramicses (the Nd of doping:YAG, rare earth volume is
1wt%).
Gained ceramic product is as shown in figure 3, Fig. 3 is the photo in kind of the gained laser ceramics of the embodiment of the present invention 1.Through surveying
Examination, the transmitance of gained potsherd is 81%；Visible according to word articulation below material object, gained ceramics transmitance is high.
Comparative example 1
(1) according to the method in embodiment 1, the accurate Y for weighing respective amount2O3、Al2O3、Nd2O3In putting ball grinder into,
A certain amount of teos is added as additive, alcohol is used as ball milling agent.The high purity aluminium oxide ball of corresponding amount is added as ball milling ball,
It is put into ball mill under the rotating speed of 240rpm, ball milling 960min.
(2) ball grinder after ball milling is put into and dries 24h in drying box in 80 DEG C, then with the screen cloth of 200 mesh to ball and
Powder is separated and the sieving to powder.
(3) powder after sieving is put into Muffle furnace and calcines 3h at 800 DEG C.
(4) by pressurize 3 minutes under the powder after calcining within the compressor 20MPa, dry-pressing formed mixing into 16mm × 16mm
Neodymium yttrium aluminium garnet element embryo.
(5) plain embryo is put into one by one after being vacuumized in vacuum bag, is put into cold etc. in 200MPa in cold isostatic press
Static pressure 3 minutes, release sampling.
(6) the plain embryo of gained after isostatic cool pressing is put into Muffle furnace and calcines 3h at 800 DEG C.
(7) by calcining after plain embryo be put into vacuum tungsten coil furnace, be raised to 1000 DEG C with the speed of 10 DEG C/min, then with 1.5
DEG C/speed of min is raised to 1750 DEG C.Insulation 10 hours, then cools to 1000 DEG C with the speed of 10 DEG C/min, treats that tungsten coil furnace is cold
But to acquisition ceramics after room temperature.
(8) ceramics annealed, polished, obtained Nd3+The YAG laser ceramicses of doping.
Gained ceramic product is as shown in figure 4, Fig. 4 is the photo in kind of the gained laser ceramics of comparative example of the present invention 1.Through surveying
Examination, the transmitance of gained potsherd is 72%.
Embodiment 2
The method and step that bait yttrium-aluminium-garnet ceramics are mixed in present invention preparation is as follows：
(1) according to mol ratio Y：Al=3:5、Er:Y=1:99, the accurate Y for weighing respective amount2O3、Al2O3、Er2O3Put
Enter in ball grinder, add a certain amount of teos as additive, alcohol is used as ball milling agent.Add the high purity aluminium oxide ball of corresponding amount
As ball milling ball, it is put into ball mill under the rotating speed of 240rpm, ball milling 960min.Wherein, teos is according to total powder quality
0.5% weighs, and alumina balls then press powder：Alcohol：Sphere volume ratio is 1：4：4 are added.
(2) ball grinder after ball milling is put into and dries 24h in drying box in 80 DEG C, then with the screen cloth of 200 mesh to ball and
Powder is separated and the sieving to powder.
(3) powder after sieving is put into Muffle furnace and calcines 3h at 800 DEG C.
(4) by pressurize 3 minutes under the powder after calcining within the compressor 20MPa, dry-pressing formed mixing into 10mm × 10mm
Yttrium-erbium-aluminum garnet element embryo.
(5) the small column voxel embryo (totally 10) of the 10mm × 10mm after will be dry-pressing formed is stacked into one one by one
Cylinder, and each two piece greatly is separated with the soft weighing scraps of paper of the circle of an Xiao Zhang 10mm × 10mm.
(6) with soft, clean preservative film (food of net purchase conventional fuse film) by the er-doped yttroalumite pomegranate of heap poststack
Stone laser ceramics element embryo is closely encased, and that is tried one's best during parcel discharges the air in sack, is repeated 3 times.
(7) after the plain embryo that will be wrapped is put into and is vacuumized in vacuum bag, it is put into cold etc. in 200MPa in cold isostatic press
Static pressure 3 minutes, release sampling.
(8) the plain embryo of gained after isostatic cool pressing is put into Muffle furnace and calcines 3h at 800 DEG C.
(9) by calcining after plain embryo be put into vacuum tungsten coil furnace, be raised to 1000 DEG C with the speed of 10 DEG C/min, then with 1.5
DEG C/speed of min is raised to 1750 DEG C, is incubated 4 hours, then cools to 1000 DEG C with the speed of 10 DEG C/min, treats that tungsten coil furnace is cold
But to acquisition ceramics after room temperature.
(10) ceramics are polished with annealing, Er is obtained3+YAG laser ceramicses (the Er of doping：YAG, rare earth volume is
1wt%).
Gained ceramic product is as shown in figure 5, Fig. 5 is the photo in kind of the gained laser ceramics of the embodiment of the present invention 2.Through surveying
Examination, the transmitance of gained potsherd is 41%.
Comparative example 2
(1) according to the method in embodiment 2, the accurate Y for weighing respective amount2O3、Al2O3、Er2O3In putting ball grinder into,
A certain amount of teos is added as additive, alcohol adds the high purity aluminium oxide ball of corresponding amount as ball milling ball as ball milling agent,
It is put into ball mill under the rotating speed of 240rpm, ball milling 960min.
(2) ball grinder after ball milling is put into and dries 24h in drying box in 80 DEG C, then with the screen cloth of 200 mesh to ball and
Powder is separated and the sieving to powder.
(3) powder after sieving is put into Muffle furnace and calcines 3h at 800 DEG C.
(4) by pressurize 3 minutes under the powder after calcining within the compressor 20MPa, dry-pressing formed mixing into 10mm × 10mm
Yttrium-erbium-aluminum garnet element embryo.
(5) plain embryo is put into one by one after being vacuumized in vacuum bag, is put into cold etc. in 200MPa in cold isostatic press
Static pressure 3 minutes, release sampling.
(6) the plain embryo of gained after isostatic cool pressing is put into Muffle furnace and calcines 3h at 800 DEG C.
(7) by calcining after plain embryo be put into vacuum tungsten coil furnace, be raised to 1000 DEG C with the speed of 10 DEG C/min, then with 1.5
DEG C/speed of min is raised to 1750 DEG C.Insulation 10 hours, then cools to 1000 DEG C with the speed of 10 DEG C/min, treats that tungsten coil furnace is cold
But to acquisition ceramics after room temperature.
(8) ceramics annealed, polished, obtained Er3+The YAG laser ceramicses of doping.
Gained ceramic product is as shown in fig. 6, Fig. 6 is the photo in kind of the gained laser ceramics of comparative example of the present invention 2.Through surveying
Examination, the transmitance of gained potsherd is 38%.
As seen from the above embodiment, the Nd that the embodiment of the present invention is sintered out using new isostatic cool pressing technology：YAG laser
Ceramic edge defect is greatly reduced, and transmitance is up to 81% after polishing.Using the method for the new isostatic cool pressing of the present invention, can be with
Prepare edge and be damaged less ceramic idiosome, and then the potsherd for preparing has transmitance higher, beneficial to application.This
Outward, operation is simple for the inventive method, and applicability is wide, is suitable to popularization and application.
The above is only the preferred embodiment of the present invention, it is noted that for making the professional technique of the art
Personnel, on the premise of the technology of the present invention principle is not departed from, are that by various modifications of these embodiments, and these
Modification also should be regarded as the scope that the present invention should be protected.
Claims (10)
1. a kind of isostatic cool pressing method suitable for optical ceramics, comprises the following steps：
A) some optical ceramics cylindrical shapes element embryo after will be dry-pressing formed is stacked into a cylinder, and each two cylinder
Separated with circular pan paper between shape element embryo；
B) cylinder for being stacked into step a) wraps up at least 2 layers with preservative film；
C) cylinder that step b) is wrapped is put into vacuum bag and is vacuumized, then isostatic cool pressing, obtain cold etc. quiet through release
Optical ceramics element embryo after pressure.
2. isostatic cool pressing method according to claim 1, it is characterised in that some optical ceramics cylindrical shapes element embryos
Number be 10~20；The height of each cylindrical shape element embryo is 10mm~30mm.
3. isostatic cool pressing method according to claim 1, it is characterised in that the circular pan paper with diameter greater than being equal to
The diameter of cylinder.
4. isostatic cool pressing method according to claim 1, it is characterised in that the circle that be stacked into for step a) by the step b)
Cylinder wraps up 3~4 layers with preservative film.
5. isostatic cool pressing method according to claim 1, it is characterised in that the pressure of the step c) isostatic cool pressings is
200MPa~250MPa, the time is 3 minutes~5 minutes.
6. isostatic cool pressing method according to claim 1, it is characterised in that the speed of the step c) releases is 20MPa/
Min~30MPa/min.
7. the isostatic cool pressing method according to any one of claim 1~6, it is characterised in that if it is described it is dry-pressing formed after
Dry optical ceramics cylindrical shape element embryo is obtained in accordance with the following methods：
Precursor powder is sequentially passed through into ball milling, sieving and is calcined, it is then dry-pressing formed, obtain some optical ceramics cylindrical shapes
Plain embryo.
8. isostatic cool pressing method according to claim 7, it is characterised in that the dry-pressing formed pressure be 20MPa~
50MPa, the time is 3 minutes~5 minutes.
9. the isostatic cool pressing method according to any one of claim 1~6, it is characterised in that the optical ceramics cylinder
Shape element embryo is to mix rare-earth yttrium-aluminium garnet element embryo, GaF2Plain embryo or Lu2O3Plain embryo.
10. a kind of preparation method of optical ceramics, comprises the following steps：
A) some optical ceramics cylindrical shapes element embryo after will be dry-pressing formed is stacked into a cylinder, and each two cylinder
Separated with circular pan paper between shape element embryo；
B) cylinder for being stacked into step a) wraps up at least 2 layers with preservative film；
C) cylinder that step b) is wrapped is put into vacuum bag and is vacuumized, then isostatic cool pressing, obtain cold etc. quiet through release
Optical ceramics element embryo after pressure；
D) by after step c) isostatic cool pressings optical ceramics element embryo calcined successively, vacuum-sintering, annealing and polish, obtain light
Learn ceramics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710073673.3A CN106799783B (en) | 2017-02-10 | 2017-02-10 | It is a kind of suitable for the isostatic cool pressing method of optical ceramics and the preparation method of optical ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710073673.3A CN106799783B (en) | 2017-02-10 | 2017-02-10 | It is a kind of suitable for the isostatic cool pressing method of optical ceramics and the preparation method of optical ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106799783A true CN106799783A (en) | 2017-06-06 |
| CN106799783B CN106799783B (en) | 2019-01-01 |
Family
ID=58987556
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710073673.3A Expired - Fee Related CN106799783B (en) | 2017-02-10 | 2017-02-10 | It is a kind of suitable for the isostatic cool pressing method of optical ceramics and the preparation method of optical ceramics |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106799783B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112692961A (en) * | 2020-12-30 | 2021-04-23 | 中鸣(宁德)科技装备制造有限公司 | Beryllium oxide ceramic cold isostatic pressing forming process |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4518546A (en) * | 1982-06-18 | 1985-05-21 | General Electric Company | Preparation of yttria-gadolinia ceramic scintillators by sintering and gas hot isostatic pressing |
| JP2005029432A (en) * | 2003-07-04 | 2005-02-03 | Pentax Corp | Method of manufacturing sintered compact and sintered compact |
| CN101249665A (en) * | 2007-01-09 | 2008-08-27 | 史考特公司 | Method for the production of optical elements and optical elements |
| 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 |
| CN105801101A (en) * | 2016-03-07 | 2016-07-27 | 武汉工程大学 | Co:ZnAl2O4 transparent ceramic as well as preparation method and application thereof |
| CN105856387A (en) * | 2015-01-19 | 2016-08-17 | 辽宁爱尔创生物材料有限公司 | Manufacturing method for zirconium dioxide ceramic green-pressing |
-
2017
- 2017-02-10 CN CN201710073673.3A patent/CN106799783B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4518546A (en) * | 1982-06-18 | 1985-05-21 | General Electric Company | Preparation of yttria-gadolinia ceramic scintillators by sintering and gas hot isostatic pressing |
| JP2005029432A (en) * | 2003-07-04 | 2005-02-03 | Pentax Corp | Method of manufacturing sintered compact and sintered compact |
| CN101249665A (en) * | 2007-01-09 | 2008-08-27 | 史考特公司 | Method for the production of optical elements and optical elements |
| 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 |
| CN105856387A (en) * | 2015-01-19 | 2016-08-17 | 辽宁爱尔创生物材料有限公司 | Manufacturing method for zirconium dioxide ceramic green-pressing |
| CN105801101A (en) * | 2016-03-07 | 2016-07-27 | 武汉工程大学 | Co:ZnAl2O4 transparent ceramic as well as preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112692961A (en) * | 2020-12-30 | 2021-04-23 | 中鸣(宁德)科技装备制造有限公司 | Beryllium oxide ceramic cold isostatic pressing forming process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106799783B (en) | 2019-01-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102924073B (en) | Method for preparing rare earth ion-doped yttrium aluminum garnet (Re: YAG) transparent laser ceramic by using hot-pressing post treatment | |
| CN103396121B (en) | Novel transparent glitter ceramic with garnet structure and preparation method thereof | |
| CN102910899B (en) | Preparation method of yttrium aluminium garnet doped transparent laser ceramics | |
| KR102391310B1 (en) | Near-infrared fluorescent powder and light-emitting device containing the fluorescent powder | |
| JP2638669B2 (en) | Ceramic body and its manufacturing method | |
| CN102020470A (en) | Preparation method of transparent yttria ceramics with high optical quality | |
| Morales-Hernández et al. | Synthesis and thermoluminescence of LaAlO3: Pr3+ to UVC radiation dosimetry | |
| CN107935581B (en) | Composite garnet scintillation ceramic with two uniformly distributed phases and preparation method thereof | |
| CN107056297A (en) | Re:Lu2O3Crystalline ceramics and its gel injection moulding preparation | |
| Luo et al. | Fabrication and spectroscopic properties of Co: MgAl2O4 transparent ceramics by the HIP post-treatment | |
| CN103058644A (en) | Method for preparing rare earth doping yttrium aluminum garnet crystalline ceramic through synthesis of rare earth doping Y2O3 nanometer powder | |
| CN108863340A (en) | A kind of composite construction transparent scintillating ceramic and preparation method thereof | |
| CN107244898A (en) | A kind of barium calcium zirconate titanate base leadless piezoelectric ceramics material of barium strontium titanate doping and preparation method thereof | |
| JP2008143726A (en) | Polycrystalline transparent y2o3 ceramics and its production method | |
| CN110183223A (en) | A kind of preparation method of crystalline ceramics | |
| Yoshida et al. | High-temperature creep resistance in lanthanoid ion-doped polycrystalline Al2O3 | |
| CN113716951A (en) | Preparation method of YAG-based transparent ceramic with large-size sheet composite structure | |
| CN104844224A (en) | Non-aqueous tape casting method for preparing laminar composite transparent ceramic | |
| CN110282650B (en) | Gadolinium oxysulfide powder for X-ray detection and preparation method of scintillation ceramic thereof | |
| CN106799783A (en) | A kind of isostatic cool pressing method and the preparation method of optical ceramics suitable for optical ceramics | |
| Zhang et al. | Preparation and characterization of transparent Tm: YAG ceramics | |
| CN101891477A (en) | Method for preparing circular rod-shaped RE:YAG laser transparent ceramics | |
| CN104944943B (en) | A kind of BNT bases no-lead electrostrictive material and preparation method with the characteristics of luminescence | |
| US20100171075A1 (en) | Scintillator having a MgAl2O4 host lattice | |
| Gan et al. | The effects of the temperature and pressure on ZrO2-doped transparent yttria ceramics fabricated by a hot-pressing method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| 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: 20190101 |