CN109574649A - A kind of preparation method of yttrium aluminum garnet transparent ceramic - Google Patents
A kind of preparation method of yttrium aluminum garnet transparent ceramic Download PDFInfo
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- CN109574649A CN109574649A CN201811536222.XA CN201811536222A CN109574649A CN 109574649 A CN109574649 A CN 109574649A CN 201811536222 A CN201811536222 A CN 201811536222A CN 109574649 A CN109574649 A CN 109574649A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 title claims abstract description 15
- 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 title claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 38
- 239000011222 crystalline ceramic Substances 0.000 claims abstract description 28
- 229910002106 crystalline ceramic Inorganic materials 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 238000001746 injection moulding Methods 0.000 claims abstract description 13
- 239000003999 initiator Substances 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- 238000007711 solidification Methods 0.000 claims description 23
- 230000008023 solidification Effects 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 19
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000001723 curing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 8
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- 239000003431 cross linking reagent Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 8
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 238000001879 gelation Methods 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000005498 polishing Methods 0.000 claims 1
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 238000000137 annealing Methods 0.000 abstract description 5
- 235000015895 biscuits Nutrition 0.000 abstract description 3
- 239000002223 garnet Substances 0.000 abstract description 2
- 238000005238 degreasing Methods 0.000 abstract 1
- 238000005266 casting Methods 0.000 description 14
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 4
- 239000005642 Oleic acid Substances 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000002513 implantation Methods 0.000 description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- QDMGKUOANLJICG-UHFFFAOYSA-N [Mg].[N+](=O)(O)[O-] Chemical compound [Mg].[N+](=O)(O)[O-] QDMGKUOANLJICG-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- -1 rare earth ion Chemical class 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 238000011415 microwave curing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004421 molding of ceramic Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 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
- C04B35/01—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
-
- 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
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/14—Producing shaped prefabricated articles from the material by simple casting, the material being neither forcibly fed nor positively compacted
-
- 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
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- 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
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63444—Nitrogen-containing polymers, e.g. polyacrylamides, polyacrylonitriles, polyvinylpyrrolidone [PVP], polyethylenimine [PEI]
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- 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
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6023—Gel casting
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- 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
- C04B2235/658—Atmosphere during thermal treatment
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- 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
Abstract
The present invention relates to a kind of preparation methods of yttrium aluminum garnet transparent ceramic, it includes the following steps: 1) powder preparation；2) it is used for the slurry preparation of gel injection-moulding；3) slurry curing is at biscuit of ceramics；4) degreasing, sintering, annealing obtain crystalline ceramics.It is characterized in that the molding mode that crystalline ceramics is selected is gel in situ curing molding mode, slurry is placed in microwave heating equipment induced curing molding in situ after catalyst and initiator are added under zero degrees celsius, heating and temperature control is within 20-60 DEG C, curing time control completes molding biscuit in 5-30 minutes, and the yttrium-aluminium-garnet curved surface crystalline ceramics for obtaining high quality is finally sintered by dumping and high temperature sintering.
Description
Technical field
The present invention relates to a kind of preparation methods of yttrium aluminum garnet transparent ceramic, belong to crystalline ceramics and prepare Material Field.
Background technique
Dangerous yttrium-aluminium-garnet (YAG) transparent ceramic material has easy-sintering because of its cubic crystal structure, and transmitance is high,
The advantages that physical and chemical performance is stablized, and thermal conductivity is high, and mechanical performance is high, good luminous performance is by as in laser lighting, fluorescence photograph
The host material in the fields such as bright, scintillator detection material, is obtained by the rare earth ion or transition metal ions that adulterate different
Excellent optical property.
The crystalline ceramics (such as lath, cylinder etc.) of simple shape can be obtained by dry-pressing formed mode, but for multiple
Miscellaneous shape, such as hemispherical, cupuliform etc. have the crystalline ceramics structure of certain sterad, and wet forming mode is preferably to select
It selects.Wet forming includes injection forming, gel casting forming, casting arrangement etc..Wherein, casting arrangement is suitble to sheet
The molding of ceramic material, the preparation including sheet composite transparent ceramic；Injection forming mode can prepare special-shaped crystalline ceramics, but by
In slip casting slurry, dehydration carries out from outside to inside in gypsum mold, easily leads to Density inhomogeneity after blank forming, is being sintered
After have serious deformation.Gel casting forming mode be by slurry inside chemical reaction formed macromolecular network structure or
Ceramic particle network structure, to make the ceramic slurry injected in mold quickly be solidified as ceramic body, relative to injection forming
There is more stable structure.But there are still many problems in current research process, firstly, gel-casting slurry is being made
It is not placed in low temperature environment during standby, easily leads to after catalyst is added with initiator and violent react occurs.Secondly solidify
Heating method not can guarantee cured consistency inside and outside slurry, such as patent CN102825649 and patent CN103553629A is
It is to be placed on gel-casting slurry in calandria at room temperature to be heating and curing by heat radiation, it is solid does not can guarantee all positions of slurry
The consistency of change process finally may result in more serious deformation in sintering shrinkage process.
Summary of the invention
For the defects in the prior art, the object of the present invention is to provide a kind of preparation sides of yttrium aluminum garnet transparent ceramic
Method.During gel casting forming, slurry is controlled in zero degrees celsius first, and play occurs after slowing down catalyst and initiator addition
The mismatch and molding non-uniform phenomenon for the local slurry that strong reaction causes.Secondly, being infused by microwave heating to gel
Deionized water heating in mould slurry, it is consistent to guarantee that solidification process green body is shunk, realize special-shaped crystalline ceramics green body molding with
It does not deform in sintering process.
The present invention is achieved by the following technical solutions:
The present invention provides a kind of preparation method of yttrium aluminum garnet transparent ceramic, it includes the following steps:
1), prepared by powder: pressing RxR’y: Y3-XAl5-yO12Weigh the Y of stoichiometric ratio2O3、Al2O3And the oxidation of Doped ions
Powder, wherein R, R ' it is doped chemical, 0≤x≤3,0≤y≤5, and according to powder: alcohol: ball=1:1:3 ratio ball milling is mixed
Even, dry, sieving obtains RxR’y: Y3-XAl5-yO12Powder；
2), note solidification forming slurry preparation: being added deionized water by solid content 50%-80% weight ratio for above-mentioned powder,
And after organic monomer Methacrylamide and crosslinking agent N, N- methylene-bisacrylamide ball milling de-bubble is added, solution is immersed in
It is maintained at zero degrees celsius in ice water, is slowly added to initiator ammonium persulfate and catalyst tetramethylethylenediamine, obtains zero degree gel
Injection molding slurry；
3) it, infuses solidification forming: above-mentioned water-based slurry is injected in spherical mould, be placed in microwave heating equipment and carry out in situ coagulate
Adhesive curing obtains gel injection moulding blank after demoulding；
4), sintering process: by above-mentioned green body dumping through the air, be sintered in vacuum and air in anneal, two-sided throwing
Spherical surface yttrium aluminum garnet transparent ceramic is obtained after light.
In above-mentioned technical proposal, the moulding process of the crystalline ceramics is that the situ-gel of aqueous based systems forms, and is formed
Journey is first to obtain uniformly mixed aluminium oxide and yttrium oxide powder, 600-900 DEG C is being calcined calcining 2-5 hours, as gel
Material powder.
According to the above scheme, organic monomer first class acrylamide in the gel rubber system: crosslinking agent N, N- methylene bisacrylamide
Amide mass ratio range is 10:1-30:1；Initiator ammonium persulfate: catalyst tetramethylethylenediamine mass ratio range is 4:
1-7:1；It is 0-10 DEG C that gel rubber system slurry keeps slurry temperature before curing.
According to the above scheme, the crystalline ceramics green body that the gel casting forming obtains uses microwave in gelation process
The mode of heating carries out heating induction in-situ solidifying molding, and curing time is 5-30 minutes.
According to the above scheme, the microwave heating temperature range is between 20 DEG C -60 DEG C.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, during gel casting forming, slurry is controlled in zero degrees celsius first, slows down catalyst and initiator is added
The mismatch and molding non-uniform phenomenon of the local slurry that violent reaction causes occur afterwards；
2, by microwave heating, the deionized water in gel-casting slurry is heated, guarantees that solidification process green body is received
Contracting is consistent, realizes that special-shaped crystalline ceramics green body does not deform in molding with sintering process.
3, guarantee the contraction of green body inner sample, gas cell distribution homogeneity in formative stage, be conducive in later period sintering process
Ceramic internal each position sintering driving force is close, reduce because local pore size extremely caused by internal porosity remain, improve
The optical property of crystalline ceramics.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is the crystalline ceramics blank of material figure of the technical solution preparation referred in the present invention；
Fig. 2, Fig. 3 are gel casting forming hemispherical CeYAG biscuit and crystalline ceramics figure；
Fig. 4 is gel injection-moulding CeYAG crystalline ceramics transmitance figure.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
A kind of preparation method of the pure YAG crystalline ceramics of hemispherical, it includes the following steps:
1), by Y3Al5O12Weigh the Y of stoichiometric ratio2O3、Al2O357.0671g and 42.8820g respectively, and weigh nitric acid
Magnesium 0.05g is as sintering aid, and oleic acid 0.5g is as dispersing agent, and according to powder: alcohol: ball=1:1:3 ratio ball milling mixes 20h,
It is dry, it is sieved 200 microns, obtains pure YAG powder；
2) deionized water, is added in 50% ratio of solid content in above-mentioned powder, and organic monomer Methacrylamide is added
After 5.00g and crosslinking agent N, N- methylene-bisacrylamide 0.40g ball milling de-bubble, solution is maintained at 10 DEG C of low temperature, slowly plus
Enter initiator ammonium persulfate 1mL and catalyst tetramethylethylenediamine 0.2mL, obtains zero degree gel-casting slurry；
3) it, by above-mentioned slurry implantation glass mold, is placed in microwave heating equipment and is solidified, solidification temperature 60
DEG C, curing time 15min continues solidification and obtains gel injection moulding blank after demoulding；
4) above-mentioned green body, is passed through into 800 DEG C of dumpings, 1800 DEG C of heat preservations vacuum-sintering in 20 hours, 1450 DEG C of annealing, two-sided throwing
YAG crystalline ceramics is obtained after light.
By the way that gel-casting slurry is cooled to zero degree, slurry slurry after initiator and catalyst is added in step 2
It is more slow to react, and is conducive to cured later and operates.At a temperature of in step 3 60 DEG C of microwave heating, solidification temperature is fast,
Solidification is completed in 5min, and subtle crackle occurs, which shows that the solidification temperature is higher, should control solidification temperature at 60 DEG C
Below.
Embodiment 2
A kind of preparation method of the pure YAG crystalline ceramics of hemispherical, it includes the following steps:
1), by Y3Al5O12Weigh the Y of stoichiometric ratio2O3、Al2O357.0671g and 42.8820g respectively, and weigh nitric acid
Magnesium 0.05g is as sintering aid, and oleic acid 0.5g is as dispersing agent, and according to powder: alcohol: ball=1:1:3 ratio ball milling mixes 20h,
It is dry, it is sieved 200 microns, obtains pure YAG powder；
2) deionized water, is added in 75% ratio of solid content in above-mentioned powder, and organic monomer Methacrylamide is added
After 5.00g and crosslinking agent N, N- methylene-bisacrylamide 0.20g ball milling de-bubble, solution is immersed in ice water keep 0 degree it is low
Temperature is slowly added to initiator ammonium persulfate 0.8mL and catalyst tetramethylethylenediamine 0.15mL, obtains zero degree gel injection-moulding slurry
Material；
3) it, by above-mentioned slurry implantation glass mold, is placed in microwave heating equipment and is solidified, solidification temperature 50
DEG C, curing time 9min continues solidification and obtains gel injection moulding blank after demoulding；
4) above-mentioned green body, is passed through into 800 DEG C of dumpings, 1800 DEG C of heat preservations vacuum-sintering in 20 hours, 1450 DEG C of annealing, two-sided throwing
YAG crystalline ceramics is obtained after light.
In embodiment 1 since microwave curing temperature is excessively high, contraction causes green body Local Cracking occur very much fastly.The present embodiment
In by the way that at a temperature of 50 DEG C of microwave heating in step 3, solidification is completed in 9min, and green body shows the solidification without craze and transfiguration phenomenon
Temperature is more suitble to, and hemispherical green body is sample in the embodiment in Fig. 1, does not observe defect, the crystalline ceramics transmitance
Reach 80%.
Embodiment 3
A kind of preparation method of hemispherical Ce:YAG crystalline ceramics, it includes the following steps:
1) Y of stoichiometric ratio, is weighed by 0.1at%Ce:YAG2O3、Al2O345.0771g and 34.1631g respectively,
CeO20.6785g simultaneously weighs magnesium nitrate 0.04g as sintering aid, and oleic acid 0.5g is as dispersing agent, and according to powder: alcohol: ball=1
: 1: 3 ratio ball milling mixes 20h, dry, is sieved 200 microns, obtains CeYAG powder；
2) deionized water, is added in 65% ratio of solid content in above-mentioned powder, and organic monomer Methacrylamide is added
After 4.00g and crosslinking agent N, N- methylene-bisacrylamide 0.22g ball milling de-bubble, solution is immersed in ice water keep 0 degree it is low
Temperature is slowly added to initiator ammonium persulfate 0.62mL and catalyst tetramethylethylenediamine 0.13mL, obtains zero degree gel injection-moulding slurry
Material；
3) it, by above-mentioned slurry implantation glass mold, is placed in microwave heating equipment and is solidified, solidification temperature 45
DEG C, curing time 11min continues solidification and obtains gel injection moulding blank after demoulding；
4) above-mentioned green body, is passed through into 800 DEG C of dumpings, 1780 DEG C of heat preservations vacuum-sintering in 15 hours, 1450 DEG C of annealing, two-sided throwing
0.1at%Ce:YAG crystalline ceramics is obtained after light.
Hemispherical Ce:YAG crystalline ceramics is successfully prepared in this embodiment, and 45 DEG C of microwave heating more appropriate, penetrates
Rate reaches 83.5%@1064nm, and still has 81.8% at 550nm, illustrates that ceramic scattering-in point is less, shows the technical side
The feasibility of case.
Embodiment 4
A kind of preparation method of hemispherical Ce:YAG crystalline ceramics, as a comparison scheme of embodiment 3, it includes such as
Lower step:
1) Y of stoichiometric ratio, is weighed by 0.1at%Ce:YAG2O3、Al2O345.0771g and 34.1631g, CeO respectively2
0.6785g simultaneously weighs magnesium nitrate 0.04g as sintering aid, and oleic acid 0.5g is as dispersing agent, and according to powder: alcohol: ball=1:1:3
Ratio ball milling mixes 20h, dry, is sieved 200 microns, obtains CeYAG powder；
2) deionized water, is added in 65% ratio of solid content in above-mentioned powder, and organic monomer Methacrylamide is added
After 4.00g and crosslinking agent N, N- methylene-bisacrylamide 0.22g ball milling de-bubble, solution is immersed in ice water keep 0 degree it is low
Temperature is slowly added to initiator ammonium persulfate 0.62mL and catalyst tetramethylethylenediamine 0.13mL, obtains zero degree gel injection-moulding slurry
Material；
3) it, by above-mentioned slurry implantation glass mold, is placed in microwave heating equipment and is solidified, solidification temperature 20
DEG C, curing time 32min continues solidification and obtains gel injection moulding blank after demoulding；
4) above-mentioned green body, is passed through into 800 DEG C of dumpings, 1780 DEG C of heat preservations vacuum-sintering in 15 hours, 1450 DEG C of annealing, two-sided throwing
1at%Nd:YAG crystalline ceramics is obtained after light.
Hemispherical Ce:YAG crystalline ceramics has equally been prepared in this embodiment, during 20 DEG C of microwave heating, slurry
Expect that solidification process declines compared with 3 medium-rate of embodiment.As shown in figure 3, compared with crystalline ceramics obtained in embodiment 3, transmitance has
Declined.Transmitance value is 81.5%@1064nm, 80.1@550nm, illustrates a small amount of scattering point occur inside ceramics, having can
It can be that solidification rate is too slow during gel casting forming, lead to phenomena such as locally generating mismatch between different powders.This is implemented
Example shows that solidification temperature may be relatively low in the technical solution.
Claims (5)
1. a kind of preparation method of yttrium aluminum garnet transparent ceramic, which is characterized in that it includes the following steps:
1), prepared by powder: pressing RxR’y: Y3-XAl5-yO12Weigh the Y of stoichiometric ratio2O3、Al2O3And the oxidate powder of Doped ions
Body, wherein R, R ' it is doped chemical, 0≤x≤3,0≤y≤5, and according to powder: alcohol: ball=1:1:3 ratio ball milling mixes, and does
Dry, sieving obtains RxR’y: Y3-XAl5-yO12Powder；
2), note solidification forming slurry preparation: deionized water is added by solid content 50%-80% weight ratio in above-mentioned powder, and is added
After entering organic monomer Methacrylamide and crosslinking agent N, N- methylene-bisacrylamide ball milling de-bubble, solution is immersed in ice water
In be maintained at zero degrees celsius, be slowly added to initiator ammonium persulfate and catalyst tetramethylethylenediamine, obtain zero degree gel injection-moulding
Slurry；
3) it, infuses solidification forming: above-mentioned water-based slurry is injected in spherical mould, it is solid to be placed in progress situ-gel in microwave heating equipment
Change, obtains gel injection moulding blank after demoulding；
4), sintering process: by above-mentioned green body dumping through the air, be sintered in vacuum and air in anneal, after twin polishing
Obtain spherical surface yttrium aluminum garnet transparent ceramic.
2. a kind of preparation method of yttrium aluminum garnet transparent ceramic as described in claim 1, which is characterized in that the transparent pottery
The moulding process of porcelain is that the situ-gel of aqueous based systems forms, and forming process is first to obtain uniformly mixed aluminium oxide and yttrium oxide
Powder is calcining 600-900 DEG C calcining 2-5 hours, the material powder as gel.
3. a kind of preparation method of yttrium aluminum garnet transparent ceramic as described in claim 1, which is characterized in that the gelinite
Organic monomer first class acrylamide in system: crosslinking agent N,N methylene bis acrylamide mass ratio range is 10:1-30:1；Draw
Send out agent ammonium persulfate: catalyst tetramethylethylenediamine mass ratio range is 4:1-7:1；Gel rubber system slurry is kept before curing
Slurry temperature is 0-10 DEG C.
4. a kind of preparation method of yttrium aluminum garnet transparent ceramic as described in claim 1, which is characterized in that the gel note
It is solid in situ that the crystalline ceramics green body that mold forming obtains carries out heating induction in gelation process by the way of microwave heating
Chemical conversion type, curing time are 5-30 minutes.
5. a kind of preparation method of yttrium aluminum garnet transparent ceramic as described in claim 1, which is characterized in that the microwave adds
Hot temperature range is between 20 DEG C -60 DEG C.
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