CN102060539A - Method for preparing yttrium aluminum garnet based transparent ceramic by slip casting - Google Patents
Method for preparing yttrium aluminum garnet based transparent ceramic by slip casting Download PDFInfo
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- CN102060539A CN102060539A CN2009101988101A CN200910198810A CN102060539A CN 102060539 A CN102060539 A CN 102060539A CN 2009101988101 A CN2009101988101 A CN 2009101988101A CN 200910198810 A CN200910198810 A CN 200910198810A CN 102060539 A CN102060539 A CN 102060539A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 53
- 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 50
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000007569 slipcasting Methods 0.000 title abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 235000015895 biscuits Nutrition 0.000 claims abstract description 45
- 238000002360 preparation method Methods 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 29
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 229910052574 oxide ceramic Inorganic materials 0.000 claims abstract description 9
- 239000011224 oxide ceramic Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 238000002347 injection Methods 0.000 claims description 28
- 239000007924 injection Substances 0.000 claims description 28
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 14
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 229920000570 polyether Polymers 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 7
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000013530 defoamer Substances 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 241000273930 Brevoortia tyrannus Species 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229910052779 Neodymium Inorganic materials 0.000 claims description 6
- 239000004902 Softening Agent Substances 0.000 claims description 6
- 235000021323 fish oil Nutrition 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- -1 polyoxyethylene Polymers 0.000 claims description 6
- 239000003125 aqueous solvent Substances 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000007704 wet chemistry method Methods 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- LGRFSURHDFAFJT-UHFFFAOYSA-N phthalic anhydride Chemical compound C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910016569 AlF 3 Inorganic materials 0.000 claims description 2
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 2
- 229910005793 GeO 2 Inorganic materials 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 125000005908 glyceryl ester group Chemical group 0.000 claims description 2
- 239000010440 gypsum Substances 0.000 claims description 2
- 229910052602 gypsum Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 claims 4
- 239000004584 polyacrylic acid Substances 0.000 claims 1
- 239000004014 plasticizer Substances 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract 2
- 230000001070 adhesive effect Effects 0.000 abstract 2
- 239000002671 adjuvant Substances 0.000 abstract 2
- 239000002518 antifoaming agent Substances 0.000 abstract 2
- 239000002270 dispersing agent Substances 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 36
- 239000011222 crystalline ceramic Substances 0.000 description 26
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 26
- 229910052799 carbon Inorganic materials 0.000 description 18
- 238000010792 warming Methods 0.000 description 16
- 238000001816 cooling Methods 0.000 description 14
- 229910006295 Si—Mo Inorganic materials 0.000 description 7
- 229910003460 diamond Inorganic materials 0.000 description 7
- 239000010432 diamond Substances 0.000 description 7
- 229960000935 dehydrated alcohol Drugs 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 239000011858 nanopowder Substances 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000010671 solid-state reaction Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000087 laser glass Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
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- 230000003335 steric effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing a yttrium aluminum garnet (YAG) based transparent ceramic by slip casting. The method comprises the following steps: performing ball-milling and mixing on oxide ceramic powder, a sintering adjuvant, a nonaqueous solvent and a dispersant; adding an adhesive, a plasticizer and a defoaming agent; and preparing a nonaqueous based slurry through ball-milling and mixing, wherein the slurry consists of the following components in percentage by mass: 40 to 70 percent of oxide ceramic powder, 0.01 to 1 percent of sintering adjuvant, 0.005 to 2.5 percent of dispersant, 0.01 to 5 percent of adhesive, 0.01 to 3 percent of plasticizer, 0.005 to 0.5 percent of defoaming agent, and the balance of the nonaqueous solvent; and preparing a ceramic block from the slurry through slip casting, preparing a ceramic biscuit by adopting a two-step drying method, and preparing the transparent ceramic through vacuum sintering. The method adopts the slip casting, is particularly suitable for preparing the ceramic sample with complicated shape, large size and composite structure, and greatly widens the preparation means of the transparent ceramic.
Description
Technical field
The present invention relates to the crystalline ceramics preparing technical field, particularly a kind of novel method of utilizing injection forming to prepare yttrium aluminum garnet (YAG) base transparent ceramic.
Background technology
Neodymium doped yttrium aluminum garnet (Nd:YAG) monocrystalline is that present performance is best, the output maximum, and the laser host material that purposes is the widest, but the natural characteristics of single crystal growing technology is restricted its performance and range of application.The material supply section scholar rises in the sixties in 20th century and just attempts with the operation material of crystalline ceramics as solid statelaser, but effect is all undesirable.Up to patent JP05-286761, JP05-286762, JP05-294722, JP05-294723, JP05-294724, after JP05-235462 etc. the issue, the ceramic laser operation material that with the Nd:YAG crystalline ceramics is representative is owing to it has monocrystalline at aspects such as technology of preparing and material properties, the glass laser material incomparable advantage has received people's very big concern, and obtained developing rapidly.
The method for preparing the Nd:YAG crystalline ceramics mainly contains two kinds: a kind of employing solid state reaction-vacuum sintering technique; Another method is to synthesize the active Nd:YAG nano-powder of high sintering with wet chemistry method earlier, adopts vacuum sintering technique to prepare the Nd:YAG crystalline ceramics then.Nineteen ninety-five, the A.Ikesue reported first with the synthetic active Y of high sintering of wet chemistry method
2O
3, Al
2O
3And Nd
2O
3Powder, adopt solid state reaction and vacuum sintering technique to prepare Nd:YAG crystalline ceramics [A.Ikesue then, T.Kinoshita, K.Kamata, et al, Fabrication and optical properties of high-performancepolycrystalline Nd:YAG ceramics for solid-state lasers, J.Am.Ceram.Soc., 1995,78 (4): 1033-1040], and first realized the continuous laser output of Nd:YAG crystalline ceramics.Wet chemistry method prepares the Nd:YAG laser ceramics and obtained important breakthrough in 1999, day Benshen island (Konoshima) chemical company adopt a kind of improved urea precipitator method prepare particle size evenly, Nd:YAG nano-powder [the patent JP10-101333 of good dispersity, JP10-101334, JP10-101411, JP10-114519], prepare high-quality Nd:YAG crystalline ceramics by vacuum sintering technique, and realized powerful laser output.
The Nd:YAG crystalline ceramics not only has the light transmission and the laser activity that can compare favourably with the laser monocrystalline, but and have the large size preparation similar and realize high-concentration dopant to laser glass, especially also have distinctive excellent high-temperature mechanical property of structural ceramics and the feature that realizes composite structure easily, so laser ceramics is considered to one of the most promising laserable material of 21 century.2006, U.S. Lao Lunsi livermore national laboratory utilizes day Nd:YAG crystalline ceramics of Benshen island chemical company production, realized the solid state heat capacity laser output of 67kW, cause showing great attention to of various countries Department of Defense, made laser ceramic material substitute the important option that the laser monocrystalline becomes US military Solid State Laser weapon.The material that uses under high-end laser weapon usefulness and the particular surroundings often needs to have characteristics such as large size, complicated shape and composite structure, adopts conventional dry-pressing formed very difficult realization.Therefore, explore the novel forming method that is fit to preparation yttrium aluminum garnet base transparent ceramic and have crucial meaning.
That injection forming is particularly suitable for preparing is complex-shaped, the sample of large size and composite structure.Injection forming and nano powder preparation technology, solid state reaction sintering technology and vacuum sintering technique are combined preparation yttrium aluminum garnet base transparent ceramic, are very promising approach.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing slip-casting shaping process to prepare the yttrium aluminum garnet base transparent ceramic, it is characterized in that the concrete processing step of this method comprises:
(1) material choice
The raw material that the present invention uses can be:
(a) α-Al
2O
3And Y
2O
3Press that YAG forms preparation or by α-Al
2O
3, Y
2O
3And RE
2O
3Press RE:YAG and form preparation, wherein RE
2O
3Be Nd
2O
3, Yb
2O
3, Cr
2O
3, Er
2O
3, Sc
2O
3, La
2O
3, Tm
2O
3, Ho
2O
3, Sm
2O
3, Lu
2O
3, Ce
2O
3And Pr
2O
3In any one or a few combination; Or (b) comprise that with wet chemical method the YAG of the precipitator method, sol-gel method, combustion synthesis method preparation or RE:YAG powder (wherein RE is any one or several combination in Nd, Yb, Cr, Er, Sc, La, Tm, Ho, Sm, Lu, Ce and the Pr element) are as oxide ceramic powder body.
(2) sintering aid is selected
Sintering aid can be LiF, NaF, MgF
2, CaF
2, AlF
3, Li
2O, Na
2O, K
2O, CaO, MgO, B
2O
3, Ga
2O
3, SiO
2, GeO
2And any one or several combination among the TEOS (tetraethoxy), the addition of sintering aid is 10
2～10
6Ppm.
(3) pulp preparation
After earlier oxide ceramic powder body, non-aqueous solvent, sintering aid and dispersion agent ball milling being mixed 6～8h, add binding agent, softening agent and defoamer, ball milling mixes 2～4h and prepares non-water-based slurry.Wherein slurry is made up of following mass percent: oxide ceramic powder body 40～70%, and sintering aid 0.01～1%, dispersion agent 0.005～1%, binding agent 0.01～5%, softening agent 0.01～3%, defoamer 0.005～0.5%, surplus is a solvent.
(4) injection forming
In mould behind the injection forming, adopt two step desiccating methods to prepare the biscuit of ceramics and the demoulding: the first step drying temperature is 20～40 ℃, and be 2～48h time of drying with the slurry of step (3) preparation; The second step drying temperature is 60～90 ℃, and drying temperature is 2～24h.
(5) ceramic post sintering
The biscuit of ceramics of step (4) preparation is carried out the pre-burning processing in retort furnace: temperature rise rate is 1～10 ℃/min, and calcined temperature is 500～1200 ℃, and soaking time is 1～10h, to get rid of the organism in the biscuit.Biscuit sintering in the vacuum tungsten coil furnace after pre-burning handled, comprising: the speed with 10～20 ℃/min is warming up to 1000 ℃ from room temperature earlier, is warming up to 1650～1850 ℃ and be incubated 1～200h with 0.5～10 ℃/min then, and the vacuum tightness during insulation is higher than 10
-3Pa.The crystalline ceramics that vacuum sintering obtains carries out anneal in air or oxygen atmosphere, annealing temperature is 1300～1600 ℃, and soaking time is 2～100h.
The purity of described raw material and sintering aid all is higher than 99.9%.
Described non-aqueous solvent is any one or the wherein several combination in methyl alcohol, ethanol, ethylene glycol, acetone, the butanone and in the dimethylbenzene.Because of the biscuit rate of drying of non-aqueous solvent preparation fast, smooth surface, microtexture is even, good mechanical performance can make the quality of crystalline ceramics be well controlled.
Described dispersion agent is any one in menhaden fish oil (MFO) polyacrylic acid (PAA) and the glyceryl ester, and these dispersion agents can be adsorbed on solid particles surface, and the space steric effect of generation can effectively stop between particle and assemble mutually.
Described binding agent is any one in polyvinyl butyral acetal (PVB) and the acrylic resin, and these two kinds of binding agents self solidify to form the three-dimensional resinous framework by the enwrapped granule surface, give the biscuit certain intensity.
Described softening agent is any one in polyoxyethylene glycol (PEG), phthalandione dibutylester (DBP) and the butyl benzyl phthalate (BBP), plasticizer molecule can be inserted in the binding agent molecular chain, thereby reduce the rigidity of binding agent molecule, improve the plasticity of biscuit of ceramics.
Described defoamer is an organic silicon modified by polyether, and this defoamer very easily is adsorbed in the liquid bubble surface, reduces the local surface tension and the surface viscosity of bubble strongly, weakens the disturbance rejection ability of bubble, destroys its stability, impels bubble to discharge liquid level.
Used ball grinder and ball milling grinding ball material is aluminum oxide or zirconia ceramics during the described ball milling of step a.
The moulding stock that injection forming is used in the described step (b) is any one in glass, gypsum, pottery, metal or the plastics.
Described injection forming be direct once shaped prepare the biscuit of one-component or repeatedly moulding preparation have the biscuit of the composite structure of layered composite structure, nucleocapsid structure.(seeing embodiment 4,5 for details)
The present invention adopts injection forming, is particularly suitable for preparing the ceramics sample of complex-shaped, large size and composite structure, has widened the preparation approach of crystalline ceramics greatly.
Description of drawings
Fig. 1 is the photo in kind of YAG crystalline ceramics among the embodiment 1
Fig. 2 is the straight line transmittance curve of YAG crystalline ceramics among the embodiment 1
Fig. 3 is the fracture apperance photo of YAG crystalline ceramics among the embodiment 1
Fig. 4 is the photo in kind of 2.0at%Nd:YAG crystalline ceramics among the embodiment 2
Fig. 5 is the straight line transmittance curve of 2.0at%Nd:YAG crystalline ceramics among the embodiment 2
Embodiment
Embodiment 1
With the 25.4904g median size is α-Al of 300nm
2O
3Powder, 33.8715g median size are the Y of 3 μ m
2O
3Powder, 0.3562g tetraethoxy (TEOS) and 0.0594g menhaden fish oil (MFO) are put into the high purity aluminium oxide ball grinder, add high purity aluminium oxide abrading-ball 200g, dehydrated alcohol 34ml, then behind the ball milling mixing 8h, after adding 0.1188g polyvinyl butyral acetal (PVB), 0.1782g polyoxyethylene glycol (PEG) and 0.1484g organic silicon modified by polyether, continue ball milling 2h, obtain the injection forming ceramic size.The slurry that makes is carried out injection forming, and the biscuit after the slip casting at 70 ℃ of dry 12h, is peeled off from mould then earlier at 30 ℃ of dry 24h, obtains the biscuit of ceramics that thickness is about 4mm.The biscuit of ceramics of preparation carries out pre-burning in retort furnace handles: temperature rise rate is 5 ℃/min, and calcined temperature is 600 ℃, and soaking time is 4h, to get rid of the organism in the biscuit.Sintering is to carry out in the vacuum tungsten coil furnace, concrete sintering mechanism is as follows: the speed with 10 ℃/min is warming up to 1000 ℃, speed with 5 ℃/min heats up 1450 ℃ then, then be warming up to 1770 ℃ and be incubated 30 hours with the speed of 2 ℃/min, speed with 10 ℃/min is cooled to 1000 ℃, furnace cooling below 1000 ℃ from 1770 ℃ then.The YAG pottery that vacuum sintering obtains anneal in the Si-Mo rod stove, mechanism of anneal is: rise to 1450 ℃ and be incubated 20h with 5 ℃/min from room temperature, then from 1450 ℃ of furnace cooling.With surface grinding machine and diamond paste pottery is carried out attenuate at last and be polished to 1.5mm thick, obtain the YAG crystalline ceramics sample of relative density＞99.9%.Fig. 1 is its photo in kind, and Fig. 2 is its straight line transmittance curve, and Fig. 3 is the microstructure appearance synoptic diagram of its fracture.
With the 25.4904g median size is α-Al of 300nm
2O
3Powder, 33.1955g median size are the Y of 3 μ m
2O
3Powder, 0.5047g median size are the Nd of 250nm
2O
3Powder, 0.3582g tetraethoxy (TEOS) and 0.0895g menhaden fish oil (MFO) are put into the high purity aluminium oxide ball grinder, add high purity aluminium oxide abrading-ball 200g, dehydrated alcohol 36ml, then behind the ball milling mixing 10h, after adding 0.2985g polyvinyl butyral acetal (PVB), 0.1194g butyl benzyl phthalate (BBP) and 0.0597g organic silicon modified by polyether, continue ball milling 2h, obtain the injection forming ceramic size.The slurry that makes is carried out injection forming, and the biscuit after the slip casting at 80 ℃ of dry 10h, is peeled off from mould then earlier at 25 ℃ of dry 24h, obtains the biscuit of ceramics that thickness is about 4mm.The biscuit of ceramics of preparation carries out pre-burning in retort furnace handles: temperature rise rate is 2.5 ℃/min, and calcined temperature is 800 ℃, and soaking time is 1h, to get rid of the organism in the biscuit.Sintering is to carry out in vacuum oven, concrete sintering mechanism is as follows: the speed with 20 ℃/min is warming up to 1000 ℃, speed with 5 ℃/min heats up 1400 ℃ then, then be warming up to 1760 ℃ and be incubated 50 hours with the speed of 2 ℃/min, speed with 20 ℃/min is cooled to 1000 ℃, furnace cooling below 1000 ℃ from 1760 ℃ then.The YAG pottery that vacuum sintering obtains anneal in the Si-Mo rod stove, mechanism of anneal is: rise to 1450 ℃ and be incubated 20h with 5 ℃/min from room temperature, then from 1450 ℃ of furnace cooling.With surface grinding machine and diamond paste pottery is carried out attenuate at last and be polished to 1.5mm thick, obtain the 2.0at%Nd:YAG crystalline ceramics sample of relative density＞99.9%.Fig. 4 is its photo in kind, and Fig. 5 is its straight line transmittance curve.
Embodiment 3
With the 25.4903g median size is α-Al of 300nm
2O
3Powder, 33.5328g median size are the Y of 3 μ m
2O
3Powder, 0.5047g median size are the Er of 7 μ m
2O
3Powder, 0.4800g tetraethoxy (TEOS) and 0.1188g polyacrylic acid (PAA) are put into the high purity aluminium oxide ball grinder, add high purity aluminium oxide abrading-ball 180g, dehydrated alcohol 30ml, behind the ball milling mixing 10h, after adding 0.0594g polyvinyl butyral acetal (PVB), 0.0594g butyl benzyl phthalate (BBP) and 0.0297g organic silicon modified by polyether, continue ball milling 2h, obtain the injection forming ceramic size.The slurry that makes is carried out injection forming, and the biscuit after the slip casting is peeled off from mould at 25 ℃ of dry 24h, obtains the biscuit of ceramics that thickness is about 3mm.The biscuit of ceramics of preparation carries out pre-burning in retort furnace handles: temperature rise rate is 2.5 ℃/min, and calcined temperature is 800 ℃, and soaking time is 2h, to get rid of the organism in the biscuit.Sintering is to carry out in vacuum oven, concrete sintering mechanism is as follows: the speed with 20 ℃/min is warming up to 1000 ℃, speed with 5 ℃/min heats up 1400 ℃ then, then be warming up to 1780 ℃ and be incubated 10 hours with the speed of 2 ℃/min, speed with 20 ℃/min is cooled to 1000 ℃, furnace cooling below 1000 ℃ from 1780 ℃ then.The YAG pottery that vacuum sintering obtains anneal in the Si-Mo rod stove, mechanism of anneal is: rise to 1450 ℃ and be incubated 20h with 5 ℃/min from room temperature, then from 1450 ℃ of furnace cooling.With surface grinding machine and diamond paste pottery is carried out attenuate at last and be polished to 1mm thick, obtain the 1at%Er:YAG crystalline ceramics sample of relative density＞99.9%.
Embodiment 4
Respectively according to embodiment 1 and two kinds of slurries of embodiment 2 preparations.The slurry that embodiment 1 is made carries out injection forming, 25 ℃ of not demouldings of dry 10h, make sizing material forming but incomplete drying, be cast in the slurry of embodiment 2 preparations top also earlier at 25 ℃ of dry 24h, at 65 ℃ of dry 10h, from mould, peel off the biscuit of ceramics that obtains layered composite structure then.The biscuit of ceramics of preparation carries out pre-burning in retort furnace handles: temperature rise rate is 5 ℃/min, and calcined temperature is 700 ℃, and soaking time is 4h, to get rid of the organism in the biscuit.Sintering is to carry out in vacuum oven, concrete sintering mechanism is as follows: the speed with 20 ℃/min is warming up to 1000 ℃, be warming up to 1760 ℃ and be incubated 20 hours with the speed of 5 ℃/min then, the speed with 20 ℃/min is cooled to 1000 ℃, furnace cooling below 1000 ℃ from 1760 ℃ then.Composite structure YAG/Nd:YAG pottery anneal in the Si-Mo rod stove that vacuum sintering obtains, mechanism of anneal is: rise to 1450 ℃ and be incubated 20h with 5 ℃/min from room temperature, then from 1450 ℃ of furnace cooling.With surface grinding machine and diamond paste pottery is carried out attenuate and polished finish at last, obtain fine and close layered composite structure YAG/Nd:YAG crystalline ceramics.
Embodiment 5
Respectively according to embodiment 1 and two kinds of slurries of embodiment 2 preparations.The slurry that embodiment 2 is made is an injection forming in the cylindrical die of 20mm at internal diameter, earlier at 25 ℃ of dry 24h, then at 65 ℃ of dry 10h, peels off from mould and obtains columniform biscuit of ceramics.This biscuit of ceramics is put in the middle of the cylindrical die that internal diameter is 50mm, the slurry that embodiment 1 is made inject columniform biscuit of ceramics around, at 25 ℃ of dry 24h, at 70 ℃ of dry 10h, from mould, peel off the biscuit of ceramics that obtains having nucleocapsid structure then earlier.According to technology pre-treatment in retort furnace successively, vacuum sintering, annealing and the polished finish of embodiment 5, finally obtain fine and close YAG/Nd:YAG crystalline ceramics then with nucleocapsid structure.
Embodiment 6
With the 25.3629g median size is α-Al of 300nm
2O
3Powder, 33.8715g median size are the Y of 3 μ m
2O
3Powder, 0.1900g median size are the Cr of about 1 μ m
2O
3Powder, 0.4457g tetraethoxy (TEOS), 0.0475g calcium oxide (CaO) powder and 0.0895g polyacrylic acid (PAA) are put into the high purity aluminium oxide ball grinder, add high purity aluminium oxide abrading-ball 200g, dehydrated alcohol 35ml, then behind the ball milling mixing 10h, after adding 0.1188g acrylic resin, 0.0594g phthalandione dibutylester (DBP) and 0.0297g organic silicon modified by polyether, continue ball milling 2h, obtain the injection forming ceramic size.The slurry that makes is carried out injection forming in glassware, the biscuit after the slip casting at 65 ℃ of dry 10h, is peeled off from mould then earlier at 25 ℃ of dry 24h, obtains the biscuit of ceramics that thickness is about 4mm.The biscuit of ceramics of preparation carries out pre-burning in retort furnace handles: temperature rise rate is 5 ℃/min, and calcined temperature is 600 ℃, and soaking time is 4h, to get rid of the organism in the biscuit.Sintering is to carry out in vacuum oven, concrete sintering mechanism is as follows: the speed with 20 ℃/min is warming up to 1000 ℃, speed with 5 ℃/min heats up 1400 ℃ then, then be warming up to 1760 ℃ and be incubated 50 hours with the speed of 2 ℃/min, speed with 20 ℃/min is cooled to 1000 ℃, furnace cooling below 1000 ℃ from 1760 ℃ then.The ceramics sample that vacuum sintering obtains is anneal in the Si-Mo rod stove, and mechanism of anneal is: rise to 1450 ℃ and be incubated 20h with 5 ℃/min from room temperature, then from 1450 ℃ of furnace cooling.With surface grinding machine and diamond paste pottery is carried out attenuate and polishes obtaining the 0.5at%Cr:YAG crystalline ceramics at last.
Embodiment 7
With the 25.3629g median size is α-Al of 300nm
2O
3Powder, 33.5328g median size are the Y of 3 μ m
2O
3Powder, the 0.1900g median size is about the Cr of 1 μ m
2O
3Powder, the 0.5911g median size is about the Yb of 5 μ m
2O
3Powder, 0.0298g calcium oxide (CaO) powder, 0.3581g tetraethoxy (TEOS) and 0.0597g menhaden fish oil (MFO) are put into the high purity aluminium oxide ball grinder, add high purity aluminium oxide abrading-ball 200g, dehydrated alcohol 36ml is then behind the ball milling mixing 10h, behind adding 0.0597g polyvinyl butyral acetal (PVB), 0.0895g polyoxyethylene glycol (PEG) and the 0.0298g organic silicon modified by polyether, continue ball milling 2h, obtain the injection forming ceramic size.The slurry that makes is carried out injection forming in glassware, the biscuit after the slip casting at 65 ℃ of dry 10h, is peeled off from mould then earlier at 25 ℃ of dry 24h, obtains the biscuit of ceramics that thickness is about 4mm.The biscuit of ceramics of preparation carries out pre-burning in retort furnace handles: temperature rise rate is 5 ℃/min, and calcined temperature is 600 ℃, and soaking time is 1h, to get rid of the organism in the biscuit.Sintering is to carry out in vacuum oven, concrete sintering mechanism is as follows: the speed with 20 ℃/min is warming up to 1000 ℃, speed with 5 ℃/min heats up 1400 ℃ then, then be warming up to 1770 ℃ and be incubated 30 hours with the speed of 2 ℃/min, speed with 20 ℃/min is cooled to 1000 ℃, furnace cooling below 1000 ℃ from 1770 ℃ then.The ceramics sample that vacuum sintering obtains is anneal in the Si-Mo rod stove, and mechanism of anneal is: rise to 1500 ℃ and be incubated 20h with 5 ℃/min from room temperature, then from 1500 ℃ of furnace cooling.With surface grinding machine and diamond paste pottery is carried out attenuate and polishes obtaining 0.5at%Cr, 1.0at%Yb:YAG crystalline ceramics at last.
Embodiment 8
Take by weighing 30g and put into the high purity aluminium oxide ball grinder with YAG nano-powder, 0.2250g tetraethoxy (TEOS) and 0.0297g menhaden fish oil (MFO) that the median size of coprecipitation method preparation is about 100nm, add high purity aluminium oxide abrading-ball 180g, dehydrated alcohol 45ml, then behind the ball milling mixing 10h, after adding 0.1188g polyvinyl butyral acetal (PVB), 0.0594g butyl benzyl phthalate (BBP) and 0.0297g organic silicon modified by polyether, continue ball milling 2h, obtain the injection forming ceramic size.The slurry that makes is carried out injection forming, and the biscuit after the slip casting at 70 ℃ of dry 12h, is peeled off from mould then earlier at 30 ℃ of dry 24h, obtains the biscuit of ceramics that thickness is about 4mm.The biscuit of ceramics of preparation carries out pre-burning in retort furnace handles: temperature rise rate is 5 ℃/min, and calcined temperature is 600 ℃, and soaking time is 4h, to get rid of the organism in the biscuit.Sintering is to carry out in vacuum oven, concrete sintering mechanism is as follows: the speed with 10 ℃/min is warming up to 1000 ℃, be warming up to 1750 ℃ and be incubated 10 hours with the speed of 2 ℃/min then, the speed with 20 ℃/min is cooled to 1000 ℃, furnace cooling below 1000 ℃ from 1750 ℃ then.The YAG pottery that vacuum sintering obtains anneal in the Si-Mo rod stove, mechanism of anneal is: rise to 1500 ℃ and be incubated 10h with 5 ℃/min from room temperature, then from 1450 ℃ of furnace cooling.With surface grinding machine and diamond paste pottery is carried out attenuate at last and be polished to 1mm thick, obtain fine and close YAG crystalline ceramics.
Claims (7)
1. a method of utilizing injection forming to prepare adulterated yttrium aluminum garnet base transparent ceramic comprises pulp preparation, injection forming, sintering and anneal, it is characterized in that:
(a) pulp preparation
Described slurry is non-water-based slurry, and its mass percent is for becoming: oxide ceramic powder body 40-70%, sintering aid 0.01-1%, dispersion agent 0.005-1%, binding agent 0.01-5%, softening agent 0.01-3%, defoamer 0.005-0.5%, surplus is a non-aqueous solvent; Oxide ceramic powder body, non-aqueous solvent, sintering aid and the mixing of dispersion agent ball milling after 6-8 hour, are added binding agent, softening agent and defoamer again, ball milling mixing 2-4 hour at first, earlier;
(b) will adopt dry preparation of two steps biscuit of ceramics after the non-water-based slurry injection forming demoulding of step a preparation, the first step drying temperature is 20-40 ℃, and second step is for 60-90 ℃;
(c) with the dried biscuit of ceramics of step b, pre-treatment under 500-1200 ℃ of temperature earlier, then at 1650-1850 ℃, vacuum sintering, vacuum tightness during sintering＞10
-3Pa;
(d) goods behind the step c sintering are annealed in 1300-1600 ℃ of air or oxygen atmosphere.
2. by the described method of claim 1, it is characterized in that described oxide ceramic powder body is:
A) α-Al
2O
3, Y
2O
3Press that YAG forms preparation or by α-Al
2O
3, Y
2O
3And RE
2O
3Press RE:YAG and form preparation; RE in the formula
2O
3Be Nd
2O
3, Yb
2O
3, Cr
2O
3, Er
2O
3, Sc
2O
3, La
2O
3, Tm
2O
3, Ho
2O
3, Sm
2O
3, Lu
2O
3, Ce
2O
3And Pr
2O
3In any one or a few combination;
B) by the YAG of wet chemistry method preparation or RE:YAG powder as oxide ceramic powder body, RE is any one or several combination in Nd, Yb, Cr, Er, Sc, La, Tm, Ho, Sm, Lu, Ce and the Pr element in the formula.
3. by the described method of claim 1, it is characterized in that:
A) described sintering aid is LiF, NaF, MgF
2, CaF
2, AlF
3, Li
2O, Na
2O, K
2O, CaO, MgO, B
2O
3, Ga
2O
3, Sc
2O
3, La
2O
3, SiO
2, GeO
2With among the TEOS any or several;
B) described solvent be in methyl alcohol, ethanol, ethylene glycol, acetone, butanone and the dimethylbenzene any or several;
C) described dispersion agent is any in menhaden fish oil, polyacrylic acid and the glyceryl ester;
D) described binding agent is a kind of in polyvinyl butyral acetal and the acrylic resin;
E) described softening agent is any in polyoxyethylene glycol, phthalandione dibutylester and the butyl benzyl phthalate;
F) described defoamer is an organic silicon modified by polyether.
4. by the described method of claim 1, used ball grinder and ball milling grinding ball material is aluminum oxide or zirconia ceramics when it is characterized in that the described ball milling of step a.
5. by the described method of claim 1, it is characterized in that:
1. the first step time of drying is 2～48h in the step (b); Be 2～24h second time of drying in step;
2. the pre-treatment soaking time is 1～10h in the step (c);
3. the sintered heat insulating time is 1～200h in the step (c);
4. the annealing soaking time is 2～100h in the step (d).
6. by the described method of claim 1, it is characterized in that injection forming is used in the described step (b) moulding stock is any one in glass, gypsum, pottery, metal or the plastics.
7. by the described method of claim 1, it is characterized in that described injection forming be direct once shaped prepare the biscuit of one-component or repeatedly the moulding preparation have the biscuit of the composite structure of layered composite structure, nucleocapsid structure.
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