CN107473728A - The preparation method of vacuum-sintering YAG base transparent ceramics under a kind of non-silicon additive - Google Patents

The preparation method of vacuum-sintering YAG base transparent ceramics under a kind of non-silicon additive Download PDF

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CN107473728A
CN107473728A CN201710803357.7A CN201710803357A CN107473728A CN 107473728 A CN107473728 A CN 107473728A CN 201710803357 A CN201710803357 A CN 201710803357A CN 107473728 A CN107473728 A CN 107473728A
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sintering
ceramics
yag
vacuum
base transparent
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张乐
周天元
邵岑
孙炳恒
高光珍
王骋
陈浩
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Jiangsu Normal University
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Abstract

The invention belongs to ceramic application and preparation technical field, and in particular to vacuum-sintering yttrium-aluminium-garnet (Y under a kind of non-silicon additive3Al5O12, YAG) base transparent ceramic method.This method is very under non-silicon additive, vacuum-sintering, using MgO and La2O3The crystalline ceramics prepared for co-sintering auxiliary agent.The present invention prepares non-silicon adjuvant system YAG crystalline ceramics using vaccum sintering process, without atmosphere auxiliary and expensive pressure sintering equipment, economical and energy saving positive effect.The present invention realizes the preparation of fine grain YAG crystalline ceramics, and grade with being reasonably distributed, grow up by crystal grain without exception.Efficiently solve silicon additive system YAG crystalline ceramics crystallite dimensions problem bigger than normal.

Description

The preparation method of vacuum-sintering YAG base transparent ceramics under a kind of non-silicon additive
Technical field
The invention belongs to ceramic application and preparation technical field, and in particular to vacuum-sintering yttroalumite pomegranate under a kind of non-silicon additive Stone (Y3Al5O12, YAG) base transparent ceramic method.
Background technology
Solid state laser with its peak power height, efficiency high, long lifespan, it is safe and reliable the advantages that, laser application lead Leading position is in domain, is widely used in fields such as defence and military, industrial processes and scientific researches.The flourishing state such as Europe, the United States at present Family supports development Solid State Laser technology with the power of country energetically, and China exists《Long-term science and technology development outline in country (2006-2020)》Also it is included among 8 big cutting edge technologies.The core component of solid state laser is gain media, and its is right The quality of output performance of laser plays conclusive effect, and therefore, carrying out further investigation to gain medium of solid laser has Highly important meaning.Gain medium of solid laser is mainly monocrystal material at present, and so it has cost height, production cycle Length, complex process, it is difficult to the defects of high concentration and Uniform Doped and large scale preparation, it is difficult to meet laser with rapid changepl. never-ending changes and improvements The demand of technology development.
Crystalline ceramics is as a kind of brand-new solid laser material, its either technology of preparing or material property etc. All there is traditional monocrystal material and the unrivaled advantage of glass material, the defects of monocrystal material can be overcome completely, development pole To be rapid, have become the focus and emphasis of laser material research, it is considered to be the laser material of future generation after monocrystal material Material.At present, various rare earth ion doped laser transparent ceramic materials emerge in an endless stream, such as yttrium-aluminium-garnet (Y3Al5O12, YAG), times The systems such as semi-oxidized thing, spinelle, fluoride, various ceramic base laser outputs are also reported in succession, and many important Preliminary Applications are obtained in field, it substitutes monocrystalline just progressively to be become a reality as gain medium of future generation.All saturating In bright ceramic material system, YAG base transparent ceramics are laser materials with advantages such as its easily prepared and good physical and chemical performances Expect the focus and emphasis of research field, have become the crystalline ceramics that achievement in research is the plentifulest and substantial, is most widely used at present Material system, development prospect are very wide.
It is well known that SiO2It is to prepare the most frequently used sintering aid of YAG crystalline ceramics.Because SiO under high temperature2Can be with YAG substrate reactions generate liquid phase, flooding mechanism is changed into liquid phase diffusion by solid-state diffusion, and it can reduce sintering temperature Diffusion rate is substantially improved simultaneously, may advantageously facilitate the densification of crystalline ceramics.However, using SiO2YAG prepared by auxiliary agent is saturating Bright ceramic crystalline grain size is generally bigger than normal, had so both been unfavorable for the mechanical performance of ceramics, and had also easily caused the transgranular gas for being difficult to exclude Hole.Other Si4+Ion generally substitutes Al in YAG lattices3+Case, its caused charge-compensation effects can greatly suppress The specific Doped ions such as high-valence state of Yb ions or Cr ions converts.Document 1 (W.Liu, J.Li, J.Liu, B.Liu, Y.Fu, Y.Pan, J.Guo, Ceram Int, 40 (2014), 8879-8883.) using tetraethyl orthosilicate, (TEOS, it is thermally decomposed into SiO2) it is that sintering aid is prepared for 0.1at.%Cr, 1.0at.%Nd:YAG crystalline ceramics, mended although with CaO as electric charge Agent is repaid, but due to Si4+Inhibitory action, Cr is almost not carried out after annealing3+→Cr4+Conversion.Drawbacks described above seriously hinders silicon The practical application of adjuvant system YAG crystalline ceramics.
In terms of the preparation of non-silicon (or few silicon) system YAG crystalline ceramics, document 2 (S.Lee, E.Kupp, A.Stevenson,J.Anderson,G.Messing,X.Li,E.Dickey,J.Dumm,V.SimonaitisCastillo, G.Quarles, J Am Ceram Soc, 92 (2009), 1456-1463.) by HIP sintering technology, by SiO2Content It is limited in 0.02wt% and is prepared for YAG crystalline ceramics, although its crystallite dimension is less than 3 μm, transmitance is about at its 1064nm 82%, the requirement of laser material can not be met.Document 3 (X.Qin, S.Hu, G.Zhou, H.Zhang, J.Zhang, and S.Wang, Rare Metal Mater Eng, 45 (2016) .240-243.) solid reaction process is used, do not helped using silicon as sintering Agent vacuum-sintering is prepared for YAG crystalline ceramics, and transmitance is 82% at its 1020nm.Document 4 (Z.Lu, T.Lu, N.Wei, B.Ma,W.Zhang,F.Li,Y.Guan,Journal of Wuhan University of Technology- Mater.Sci.Ed., 28 (2013), 320-324.) use coprecipitation technology combination vacuum sintering technique.In non-silicon additive condition Under be prepared for Yb:YAG crystalline ceramics, its transmitance only 80.6% at 1100nm；Although document 5 (Z.Lu, T.Lu, N.Wei, W.Zhang, B.Ma, J.Qi, Y.Guan, X.Chen, H.Wu, Y.Zhao, Opt Mater, 47 (2015), 292-296.) pass through The technology of preparing of document 4 is improved, by vacuum-sintering combination HIP sintering technology by transmitance at the ceramic 1100nm 83.5% is promoted to, but still has certain gap away from theoretical transmission.
The non-silicon adjuvant system YAG base transparent ceramics that document above is reported in the prevalence of transmitance it is relatively low the problems such as, Far away from the optical quality of YAG monocrystalline, Solid State Laser application demand can not be met, it is main reason is that relative to silicon additive body System, non-silicon adjuvant system are more difficult to promote the densification of YAG crystalline ceramics, are unfavorable for being lifted the optical quality of crystalline ceramics.To the greatest extent Pipe can provide extra densification for ceramic post sintering relative to vacuum-sintering, HIP sintering technology by impressed pressure Change driving force, but HIP sintering, relative to vacuum-sintering, its high-pressure sinter environment is very high to equipment requirement, is unfavorable for saving The about energy, and there is certain risk.So far, this area is not yet developed using non-silicon adjuvant system directly in vacuum bar Being prepared under part has good optical qualities fine grain YAG base transparent ceramic materials and preparation method thereof.
Therefore, this area can meet Solid State Laser application demand, the effectively save energy of and can there is an urgent need to develop one kind The method that the YAG base transparent ceramic materials with good optical qualities are prepared under the non-silicon additive in source.
The content of the invention
For it is existing the problem of, the invention provides a kind of vacuum-sintering prepare non-silicon adjuvant system YAG base transparent ceramics Method, so as to solve the problems, such as that prior art is present.This method technique is simple, it is not necessary to high-tension apparatus costly, Prepared crystalline ceramics crystallite dimension is tiny, and 1.8~5.9 μm, particle diameter distribution is uniform, excellent in optical properties, and its 1064nm is saturating Rate is crossed higher than 84.1%, can be used as gain medium of solid laser.
The present invention is achieved through the following technical solutions：
The invention provides a kind of method for preparing YAG base transparent ceramics, under non-silicon additive, vacuum-sintering, using MgO And La2O3The crystalline ceramics prepared for co-sintering auxiliary agent, component meet following formula:
(RexY1-x)3(CryAl1-y)5O12
X scope takes 0≤x≤0.3 in formula, and y scope takes 0≤y≤0.003, Re Nd, Yb, Er, Ho, Dy, Pr, Tm, Sm, Eu or Tb one kind；The total addition level of sintering aid is the 0.05%~0.50% of Y-ion molal quantity, wherein La and Mg's Mol ratio is La/Mg=1:4~1:1.
Further, above-mentioned preparation method comprises the following steps：
Step 1, raw material are chosen：Al raw materials are purity 99.99% and above α-Al2O3Powder, Y raw materials are purity 99.99% and above Y2O3Powder, Cr raw materials are purity 99.99% and above Cr2O3Powder, Re raw materials be purity 99.99% and Above Re2O3Powder；After above-mentioned raw materials powder is weighed by the stoichiometric proportion of required metallic element, it is placed in ball grinder, and Add sintering aid, dispersant and absolute ethyl alcohol configuration slurry；
Step 2, ball milling sieving：The slurry that step 1 configures is placed in 6~18h of ball milling in ball mill, received using evaporating dish Collect the ethanol based sizing after ball milling, be placed in baking oven drying 10-48 hours, dried slurry grinding at 40~120 DEG C Sieving；
Step 3：Forming of green body：By in step 2 sieve after powder be placed in stainless steel mould, 10Mpa~ Dry-pressing formed under 100Mpa pressure, the biscuit after dry-pressing is subsequently placed in hermetic bag, using cold under 100Mpa~300Mpa pressure Isostatic pressing.Biscuit of ceramics after shaping is placed in Muffle furnace, using 350~1000 DEG C of 2~15h of calcining, and is cooled to 20 ~40 DEG C；
Step 4：Sintering：Will in step 3 calcining removal of impurities after biscuit of ceramics be placed in vacuum drying oven using 1700 DEG C~ 1850 DEG C of 2~50h of vacuum-sintering, are then cooled to 30~50 DEG C, obtain non-silicon additive YAG base transparent ceramic materials.
Further, the line transmitance at 1064nm of the YAG transparent ceramic materials prepared by the present invention is higher than 84.1, thickness For 2~4mm；Ceramic crystalline grain size is 1.8~5.9 μm.
Further, the ball grinder in above-mentioned steps one is high purity aluminium oxide ball grinder；Sintering aid is La2O3And MgO； The dispersant is DS005, and its addition is 0.1~1wt% of Y, Al raw material silty amount summation；Final configuration slurry solid content For 30%~65%.
Further, the ball milling method in above-mentioned steps two is planetary ball mill, and abrading-ball uses high purity aluminium oxide ball, ball mill Rotating speed is 120~280r/min；Dried powder sieves 1~4 time, and screen number is 50~200 mesh.
Further, the dwell time of the cold isostatic compaction in above-mentioned steps three is 1~20min；Calcine heating rate For 0.5-10 DEG C/min, rate of temperature fall is 5~20 DEG C/min, and calcination atmosphere is air atmosphere or oxygen atmosphere.
Further, the sintering vacuum in above-mentioned steps four is higher than 10-3Pa, sintering heating rate be 0.5-10 DEG C/ Min, rate of temperature fall are 2~50 DEG C/min；The heating rate of annealing is 1~30 DEG C/min, and rate of temperature fall is 1~50 DEG C/min, The machining includes that frosted is thinned and polishing.
Beneficial technique effect：
La ions are mixed in YAG matrix, due to La ions, segregation coefficient is relatively low in YAG lattices, and relative to other Cation for additive has higher atomic mass, so advantageously passes through its " pricking nail to act on " to crystal boundary in it Suppress crystal boundary migration, control the too fast growth of crystal grain, it is tiny to be readily available crystal grain, the uniform microstructure of ceramics of particle diameter distribution, with Ceramic optical loss is reduced, strengthens ceramic machinery performance, while more crystal boundary excludes to provide more passages for stomata. Mg ions are mixed in YAG matrix, due to Mg2+Ionic radius and Al3+Close, it is easy to substitute in YAG lattices in sintering process Regular octahedron Al3+Case, it can lift diffusion coefficient effectively at sintering by vacancy mechanism, be advantageous to ceramics and sintering During stomata exclusion, promote ceramic densifying, reduce scattering loss, lift its optical quality, while may advantageously facilitate one High-valence state conversion (such as Cr of a little specific foreign atoms3+→Cr4+,Yb2+→Yb3+).In addition, Mg auxiliary agents can be at 1540 DEG C extremely Promote grain growth and the densification of ceramics in 1660 DEG C of temperature ranges., can be effective so under relatively low densification temperature Ground expands densification temperature section, promotes sintering and the densification of ceramics, obtains consistency height, and the YAG of excellent in optical properties is saturating Bright ceramics.Finally, Mg and La ions may generate fluxing phase with Al ionic reactions in YAG matrix, can further promote YAG saturating Bright ceramic densification.Finally, La3+And Mg2+May be with Al in YAG matrix3+Reaction generates fluxing phase, two kinds of ion collaborations Fluxing action, further promote the densification of YAG crystalline ceramics.
Based on it is above-mentioned the characteristics of, summarize the present invention advantage it is as follows：
(1) present invention uses solid reaction process combination vacuum sintering technique to realize high quality YAG bases under non-silicon additive saturating Bright ceramic preparation, prepared ceramic dense degree is high, uniformity is good, segregation-free, without transgranular and intergranular stomata, transmitance Height, meet the condition as gain medium.
(2) present invention prepares non-silicon adjuvant system YAG crystalline ceramics using vaccum sintering process, without atmosphere auxiliary and costliness Pressure sintering equipment, economical and energy saving positive effect.
(3) present invention realizes the preparation of fine grain YAG crystalline ceramics, and grade with being reasonably distributed, grow up by crystal grain without exception. Efficiently solve silicon additive system YAG crystalline ceramics crystallite dimensions problem bigger than normal.
(4) technological process is simple, short preparation period, advantageously reduces cost requirement, realizes Technique Popularizing and business promotion.
Brief description of the drawings
Fig. 1：The XRD spectrum of the YAG base transparent ceramics described in 2,3,4,5, it is pure YAG phases according to embodiment 1.
Fig. 2：Scheme according to the YAG base transparent ceramic polished surfaces SEM described in embodiment Isosorbide-5-Nitrae, it is complete to show that the ceramics have Densified structure, crystallite dimension is tiny.
Fig. 3：According to the line transmittance curve of the YAG base transparent ceramics described in embodiment Isosorbide-5-Nitrae, it is higher to show that the ceramics have Optical quality.
Fig. 4：According to the light microscope bright field image of the YAG base transparent ceramics described in embodiment 4, illustrate that the ceramics have Good optical homogeneity.
Fig. 5：According to the transmitance collection of illustrative plates after the YAG base transparent ceramics annealing described in embodiment 1 and absorb collection of illustrative plates.
Fig. 6：According to the photo in kind of the YAG base transparent ceramics described in embodiment 1,4.
Embodiment
Embodiment 1#：
1. by the Y that commercial concentration is 99.999%2O3, 99.999% Al2O3With 99.999% Cr2O3By Y3 (Cr0.003Al0.997)5O12After stoichiometric proportion weighs, it is placed in ball grinder, then adds 0.20mol%La2O3With 0.20mol%MgO is configured to solid content and is as sintering aid, 0.3wt%DS005 as dispersant, addition absolute ethyl alcohol 40% slurry.
2. by step 1. in obtained slurry be placed in ball milling mixing 10 hours on planetary ball mill, rotating speed 220r/ Min, the slurry after ball milling, which is placed at 50 DEG C, dries 36h, and dried presoma is sieved, and is sieved 3 times using 80 mesh mesh screens.
3. by step, 2. resulting sieving powder is placed in stainless steel mould, and disk is pressed into using 60Mpa dry-pressing, then Biscuit, dwell time 15min is made by 180MPa isostatic cool pressings.Biscuit is in air atmosphere using 700 DEG C of calcinings, insulation 6 hours, and it is cooled to 20 DEG C.Calcining heating rate is 5 DEG C/min, 5 DEG C/min of rate of temperature fall.
4. the biscuit after step 3. resulting calcining is placed in vacuum sintering furnace, using 1800 DEG C of vacuum-sintering 20h, Vacuum is 10-4Pa, then it is cooled to 30 DEG C.1.5 DEG C/min of heating rate is sintered, 20 DEG C/min of rate of temperature fall, obtains densification YAG crystalline ceramics, and frosted, be polished to 3mm thickness.The XRD spectrum (Bruker D2) of ceramics sample is shown in Fig. 1, is pure YAG phases； The polished surface collection of illustrative plates (JEOL, JSM6510) of sample is shown in Fig. 2, shows that the ceramics have complete densification microstructure, no gas Hole and intergranular are mutually present, and average grain size is 2.4 μm；The line transmitance collection of illustrative plates (Lambda 950, Perkin of sample Elmer Fig. 3) is seen, line transmitance is 84.7% at its 1064nm, reaches YAG theoretical transmissions, shows that sample has good light Learn quality；Sample is dropped then with 1 DEG C/min heating rates in 1300 DEG C of air atmospheres annealing 5h with 1 DEG C/min rate of temperature fall To 20 DEG C.Transmitance collection of illustrative plates and absorption collection of illustrative plates are shown in Fig. 5 after sample annealing, and transmitance reaches YAG up to 85.4% at its 1500nm Theoretical transmission, its at 1030nm absorption coefficient up to 3.8cm-1, far above monocrystalline, show its have sufficient tetravalence chromium from Sub- transformation efficiency；The pictorial diagram of sample after annealing is shown in Fig. 6.
Embodiment 2#：
1. by the Y that commercial concentration is 99.99%2O3, 99.99% Al2O3, 99.99% Nd2O3With 99.99 Cr2O3 By (Nd0.01Y0.99)3(Cr0.001Al0.999)5O12After stoichiometric proportion weighs, it is placed in ball grinder, then adds 0.02mol% La2O3It is configured to solid content as dispersant, addition absolute ethyl alcohol as sintering aid, 1wt%DS005 with 0.03molMgO and is 30% slurry.
2. by step 1. in obtained slurry be placed in ball milling mixing 6 hours on planetary ball mill, rotating speed 280r/min, Slurry after ball milling, which is placed at 120 DEG C, dries 10h, and dried presoma is sieved, and is sieved 4 times using 50 mesh mesh screens.
3. by step, 2. resulting sieving powder is placed in stainless steel mould, and disk is pressed into using 100Mpa dry-pressing, Biscuit, dwell time 20min is made by 100MPa isostatic cool pressings again.Biscuit, using 350 DEG C of calcinings, is protected in oxygen atmosphere Temperature 15 hours, and it is cooled to 30 DEG C.Calcining heating rate is 10 DEG C/min, 20 DEG C/min of rate of temperature fall.
4. the biscuit after step 3. resulting calcining is placed in vacuum sintering furnace, using 1850 DEG C of vacuum-sintering 2h, Vacuum is 10-3Pa, then it is cooled to 40 DEG C.10 DEG C/min of heating rate, 50 DEG C/min of rate of temperature fall are sintered, obtains densification YAG crystalline ceramics, and frosted, be polished to 2mm thickness.The XRD spectrum (Bruker D2) of ceramics sample is shown in Fig. 1, is pure YAG phases；It is flat Equal crystallite dimension is 1.8 μm, and line transmitance is 84.1% at 1064nm；Sample is then with 30 DEG C/min heating rates in 1200 DEG C Oxygen atmosphere annealing 20h, and it is down to 30 DEG C with 50 DEG C/min rate of temperature fall.After annealing, transmitance is reachable at sample 1500nm 85.0%, reach YAG theoretical transmissions, its at 1030nm absorption coefficient up to 3.2cm-1, far above monocrystalline, show that sample has There is sufficient tetravalence chromium ion transformation efficiency.
Embodiment 3#：
1. by the Y that commercial concentration is 99.999%2O3, 99.999% Al2O3With 99.999% Yb2O3Press (Yb0.3Y0.7)3Al5O12After stoichiometric proportion weighs, it is placed in ball grinder, then adds 0.25mol%La2O3And 0.25mol% MgO adds absolute ethyl alcohol and is configured to the slurry that solid content is 65% as sintering aid, 0.1wt%DS005 as dispersant.
2. by step 1. in obtained slurry be placed in ball milling mixing 18 hours on planetary ball mill, rotating speed 120r/ Min, the slurry after ball milling, which is placed at 40 DEG C, dries 48h, and dried presoma is sieved, and 1 is sieved using 200 mesh mesh screens It is secondary.
3. by step, 2. resulting sieving powder is placed in stainless steel mould, and disk is pressed into using 40Mpa dry-pressing, then Biscuit, dwell time 5min is made by 250MPa isostatic cool pressings.Biscuit is in air atmosphere using 1000 DEG C of calcinings, insulation 2 hours, and it is cooled to 40 DEG C.Calcining heating rate is 8 DEG C/min, 15 DEG C/min of rate of temperature fall.
4. the biscuit after step 3. resulting calcining is placed in vacuum sintering furnace, using 1700 DEG C of vacuum-sintering 50h, Vacuum is 10-5Pa, then it is cooled to 50 DEG C.3 DEG C/min of heating rate, 10 DEG C/min of rate of temperature fall are sintered, obtains densification YAG crystalline ceramics, and frosted, be polished to 4mm thickness.The XRD spectrum (Bruker D2) of ceramics sample is shown in Fig. 1, is pure YAG phases；It is flat Equal crystallite dimension is 5.1 μm, and line transmitance is 84.2% at 1064nm；Sample is then with 20 DEG C/min heating rates in 1450 DEG C Air atmosphere annealing 15h, and it is down to 50 DEG C with 30 DEG C/min rate of temperature fall.Transmitance is reachable at sample 1064nm after annealing 84.4%, reach YAG theoretical transmissions, and fully achieve Yb2+→Yb3+Conversion.
Embodiment 4#：
1. by the Y that commercial concentration is 99.999%2O3With 99.999% Al2O3By Y3Al5O12After stoichiometric proportion weighs, It is placed in ball grinder, then adds 0.07mol%La2O3With 0.28mol%MgO as sintering aid, 0.5wt%DS005 conducts Dispersant, add absolute ethyl alcohol and be configured to the slurry that solid content is 50%.
2. by step 1. in obtained slurry be placed in ball milling mixing 15 hours on planetary ball mill, rotating speed 180r/ Min, the slurry after ball milling, which is placed at 70 DEG C, dries 24h, and dried presoma is sieved, and 3 are sieved using 100 mesh mesh screens It is secondary.
3. by step, 2. resulting sieving powder is placed in stainless steel mould, and disk is pressed into using 80Mpa dry-pressing, then Biscuit, dwell time 10min is made by 2000MPa isostatic cool pressings.Biscuit, using 850 DEG C of calcinings, is protected in air atmosphere Temperature 4 hours, and it is cooled to 30 DEG C.Calcining heating rate is 0.5 DEG C/min, 10 DEG C/min of rate of temperature fall.
4. the biscuit after step 3. resulting calcining is placed in vacuum sintering furnace, using 1820 DEG C of vacuum-sintering 8h, Vacuum is 10-6Pa, then it is cooled to 30 DEG C.Sinter 0.5 DEG C/min of heating rate, 30 DEG C/min of rate of temperature fall.Sample without Cross annealing.Obtain densification YAG crystalline ceramics, and frosted, be polished to 3mm thickness.XRD spectrum (the Bruker of ceramics sample D2) see Fig. 1, be pure YAG phases；The polished surface collection of illustrative plates (JEOL, JSM6510) of sample is shown in Fig. 2, and it is complete to show that the ceramics have Microstructure is densified, pore-free and intergranular are mutually present, and average grain size is 4.9 μm；Sample transmitance collection of illustrative plates (Lambda 950, Perkin elmer) see Fig. 3, its transmitance at 1064nm up to 84.5%, reaches YAG theoretical transmissions；Sample Light microscope collection of illustrative plates (Carl Zssis, Axio Scope.A1) is shown in Fig. 4, illustrates that it has good optical homogeneity；Sample Pictorial diagram see Fig. 6.
Embodiment 5#：
1. by the Y that commercial concentration is 99.999%2O3, 99.999% Al2O3, 99.999% Yb2O3With 99.999 Cr2O3By (Yb0.1Y0.9)3(Cr0.002Al0.998)5O12After stoichiometric proportion weighs, it is placed in ball grinder, then adds 0.1mol%La2O3With 0.3mol%MgO absolute ethyl alcohol configuration is added as sintering aid, 0.8wt%DS005 as dispersant Into the slurry that solid content is 60%.
2. by step 1. in obtained slurry be placed in ball milling mixing 12 hours on planetary ball mill, rotating speed 240r/ Min, the slurry after ball milling, which is placed at 90 DEG C, dries 20h, and dried presoma is sieved, and 2 are sieved using 150 mesh mesh screens It is secondary.
3. by step, 2. resulting sieving powder is placed in stainless steel mould, and disk is pressed into using 10Mpa dry-pressing, then Biscuit, dwell time 1min is made by 300MPa isostatic cool pressings.Biscuit is in air atmosphere using 600 DEG C of calcinings, insulation 10 hours, and it is cooled to 20 DEG C.Calcining heating rate is 3 DEG C/min, 8 DEG C/min of rate of temperature fall.
4. the biscuit after step 3. resulting calcining is placed in vacuum sintering furnace, using 1750 DEG C of vacuum-sintering 20h, Vacuum is 10-6Pa, then it is cooled to 40 DEG C.2 DEG C/min of heating rate, 2 DEG C/min of rate of temperature fall are sintered, obtains densification YAG crystalline ceramics, and frosted, be polished to 3mm thickness.The XRD spectrum (Bruker D2) of ceramics sample is shown in Fig. 1, is pure YAG phases.Sample Product average grain size is 5.9 μm, and line transmitance is 84.4% at 1064nm；Sample then with 10 DEG C/min heating rates in 1300 DEG C of air atmospheres annealing 10h, and it is down to 20 DEG C with 40 DEG C/min rate of temperature fall.Transmitance can at sample 1500nm after annealing Up to 85.2%, reach YAG theoretical transmissions, its at 1030nm absorption coefficient up to 3.5cm-1, far above monocrystalline, show sample With sufficient tetravalence chromium ion transformation efficiency.

Claims (7)

  1. A kind of 1. method for preparing YAG base transparent ceramics, it is characterised in that under non-silicon additive, vacuum-sintering, using MgO and La2O3The crystalline ceramics prepared for co-sintering auxiliary agent, component meet following formula:
    (RexY1-x)3(CryAl1-y)5O12
    X scope takes 0≤x≤0.3 in formula, and y scope takes 0≤y≤0.003, Re Nd, Yb, Er, Ho, Dy, Pr, Tm, Sm, Eu or Tb one kind；The total addition level of sintering aid is mole of the 0.05%~0.50% of Y-ion molal quantity, wherein La and Mg Than for La/Mg=1:4~1:1.
  2. 2. the method according to claim 1 for preparing YAG base transparent ceramics, it is characterised in that comprise the following steps：
    Step 1, raw material are chosen：Al raw materials are the α-Al of purity 99.99% and the above2O3Powder, Y raw materials are purity 99.99% And the Y of the above2O3Powder, Cr raw materials are the Cr of purity 99.99% and the above2O3Powder, Re raw materials be purity 99.99% and with On Re2O3Powder；After above-mentioned raw materials powder is weighed by the stoichiometric proportion of required metallic element, it is placed in ball grinder, and Add sintering aid, dispersant and absolute ethyl alcohol configuration slurry；
    Step 2, ball milling sieving：The slurry that step 1 configures is placed in 6~18h of ball milling in ball mill, ball is collected using evaporating dish Ethanol based sizing after mill, it is placed in baking oven drying 10-48 hours, dried slurry grinding sieving at 40~120 DEG C；
    Step 3：Forming of green body：Powder after being sieved in step 2 is placed in stainless steel mould, pressed in 10Mpa~100Mpa Dry-pressing formed under power, the biscuit after dry-pressing is subsequently placed in hermetic bag, using isostatic cool pressing under 100Mpa~300Mpa pressure into Type；Biscuit of ceramics after shaping is placed in Muffle furnace, using 350~1000 DEG C of 2~15h of calcining, and is cooled to 20~40 DEG C；
    Step 4：Sintering：Biscuit of ceramics after calcining removal of impurities in step 3 is placed in vacuum drying oven and uses 1700 DEG C~1850 DEG C 2~50h of vacuum-sintering, 30~50 DEG C are then cooled to, obtain non-silicon additive YAG base transparent ceramic materials.
  3. 3. the method for preparing YAG base transparent ceramics according to right 2, it is characterised in that the transparent potteries of YAG of described preparation Ceramic material line transmitance at 1064nm is higher than 84.1, and thickness is 2~4mm；Ceramic crystalline grain size is 1.8~5.9 μm.
  4. 4. the method according to claim 2 for preparing YAG base transparent ceramics, it is characterised in that in described step one Ball grinder is high purity aluminium oxide ball grinder；Sintering aid is La2O3And MgO；The dispersant is DS005, and its addition is Y, Al 0.1~1wt% of raw material silty amount summation；Final configuration slurry solid content is 30%~65%.
  5. 5. the method according to claim 2 for preparing YAG base transparent ceramics, it is characterised in that in described step two Ball milling method is planetary ball mill, and abrading-ball uses high purity aluminium oxide ball, and drum's speed of rotation is 120~280r/min；Dried powder Body sieves 1~4 time, and screen number is 50~200 mesh.
  6. 6. the method according to claim 2 for preparing YAG base transparent ceramics, it is characterised in that in described step three The dwell time of cold isostatic compaction is 1~20min；Calcining heating rate is 0.5-10 DEG C/min, and rate of temperature fall is 5~20 DEG C/min, calcination atmosphere is air atmosphere or oxygen atmosphere.
  7. 7. the method according to claim 2 for preparing YAG base transparent ceramics, it is characterised in that in described step four Sinter vacuum and be higher than 10-3Pa, sintering heating rate are 0.5-10 DEG C/min, and rate of temperature fall is 2~50 DEG C/min；The liter of annealing Warm speed is 1~30 DEG C/min, and rate of temperature fall is 1~50 DEG C/min, and the machining includes that frosted is thinned and polishing.
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