CN107129293A - A kind of preparation method of Mg adjuvant systems YAG base transparent ceramics - Google Patents
A kind of preparation method of Mg adjuvant systems YAG base transparent ceramics Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims description 14
- 239000002671 adjuvant Substances 0.000 title abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 70
- 229910002106 crystalline ceramic Inorganic materials 0.000 claims abstract description 45
- 239000011222 crystalline ceramic Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000000137 annealing Methods 0.000 claims abstract description 20
- 230000007246 mechanism Effects 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 36
- 239000002994 raw material Substances 0.000 claims description 28
- 239000002002 slurry Substances 0.000 claims description 28
- 235000015895 biscuits Nutrition 0.000 claims description 27
- 238000001354 calcination Methods 0.000 claims description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 22
- 238000000498 ball milling Methods 0.000 claims description 22
- 239000012752 auxiliary agent Substances 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 19
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 229910052727 yttrium Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 229910010293 ceramic material Inorganic materials 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005056 compaction Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 238000003754 machining Methods 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 239000004677 Nylon Substances 0.000 claims description 4
- 239000001095 magnesium carbonate Substances 0.000 claims description 4
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 229910052702 rhenium Inorganic materials 0.000 claims description 4
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052689 Holmium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910019599 ReO2 Inorganic materials 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 238000007493 shaping process Methods 0.000 claims description 3
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 30
- 239000002223 garnet Substances 0.000 abstract description 5
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 62
- 238000000280 densification Methods 0.000 description 20
- 239000000463 material Substances 0.000 description 16
- 238000005516 engineering process Methods 0.000 description 10
- 238000003825 pressing Methods 0.000 description 10
- 238000001228 spectrum Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 5
- 229910001425 magnesium ion Inorganic materials 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 239000000306 component Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007717 exclusion Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
What the present invention was provided one kind prepares yttrium-aluminium-garnet (Y under non-annealing mechanism based on vacuum-sintering under a small amount of Mg single fires knot adjuvant system3Al5O12, YAG) base transparent ceramic method, using a small amount of Mg as single sintering aid, using single step vaccum sintering process, in the case where being not added with making annealing treatment with the later stage, prepare the YAG crystalline ceramics with good optical qualities and fine grain size.
Description
Technical field
The invention belongs to advanced ceramics preparation field, it is related to a kind of preparation method of Mg adjuvant systems YAG base transparent ceramics,
Specifically related to one kind prepares yttrium-aluminium-garnet (Y under non-annealing mechanism based on the mono- auxiliary agent body vacuum-sinterings of a small amount of Mg3Al5O12,
YAG) the method for base transparent ceramic.
Background technology
Solid state laser with its peak power height, efficiency high, long lifespan, it is safe and reliable the advantages of, laser application neck
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 current Europe, the United States
Family supports development Solid State Laser technology energetically with the power of country, 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, therefore, and carrying out further investigation to gain medium of solid laser has
Highly important meaning.Current gain medium of solid laser is mainly monocrystal material, and so it has cost height, production cycle
Length, complex process, it is difficult to high concentration and Uniform Doped and large scale and the defect such as prepares, it is difficult to meets 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, and it is either in terms of technology of preparing or material property
All there is traditional monocrystal material and the unrivaled advantage of glass material, the defect of monocrystal material, development pole can be overcome completely
To be rapid, the focus and emphasis of laser material research is had become, 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 replaces 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, with advantages such as its easily prepared and good physical and chemical performances, are laser materials
Expect the focus and emphasis of research field, the crystalline ceramics that achievement in research is the plentifulest and substantial, be most widely used is had become at present
Material system, development prospect is very wide.
In terms of the preparation of YAG crystalline ceramics, densification completely is realize YAG crystalline ceramics good optical qualities basic
It is required that.Therefore in order to further lift the final optical quality of YAG crystalline ceramics, it will usually sinter additives are introduced, that is, are sintered
Auxiliary agent.The purpose of sintering aid is the densification of further promotion ceramics, while the number of scattering source (such as hole) can be reduced
Mesh, and the fast transferring of crystal boundary can be prevented in sintering process, suppress the formation of transgranular stomata, be conducive to acquisition crystal grain thin
It is small, it is evenly distributed and complete fully dense microstructure of ceramics, lifts its optical property.
It is well known that tetraethyl orthosilicate (TEOS) is to prepare the most frequently used sintering aid of YAG crystalline ceramics.Because high
The lower TEOS of temperature is thermally decomposed to generate SiO2, it can generate liquid phase with YAG substrate reactions, flooding mechanism is changed into by solid-state diffusion
Liquid phase spreads, and diffusion rate can be substantially improved while sintering temperature is reduced in it, may advantageously facilitate the densification of crystalline ceramics
Change.However, the YAG crystalline ceramics crystallite dimension prepared using TEOS auxiliary agents is generally bigger than normal, the machinery of ceramics so both it had been unfavorable for
Performance, also easily causes the transgranular stomata for being difficult to exclude.
Mg auxiliary agents are relative to TEOS auxiliary agents, because Mg2+Ionic radius and YAG lattices in hexa-coordinate Al3+Ionic radius phase
Closely, with higher solid solubility, therefore it can lift diffusion coefficient effectively by vacancy mechanism, be conducive to ceramics burning
The exclusion of stomata during knot, lifts its optical quality, reduces scattering loss.In addition, Mg with its+2 valence property, be conducive to promote
Enter high-valence state conversion (such as Cr of some specific foreign atoms3+→Cr4+,Yb2+→Yb3+) Mg auxiliary agents can be in relatively low burning
Junction temperature (being less than 1660 DEG C) promotes the densification of YAG crystalline ceramics, and can be between 1540 DEG C and 1660 DEG C of sintering temperature
Promote grain growth.Under relatively low densification temperature, it can effectively expand densification temperature interval, promote the sintering of ceramics
And densification, be conducive to further excluding scattering center, with reference to non-annealing mechanism, scattering loss can be effectively reduced, obtain
Consistency is high, the YAG crystalline ceramics of excellent in optical properties.Other Mg auxiliary agents are relative to Ca auxiliary agents, because Ca auxiliary agents are in YAG lattices
In solid solubility there was only 300~400ppm, therefore easily cause segregation, aggravate optical loss.
In terms of Mg adjuvant systems prepare the preparation of YAG crystalline ceramics, document 1 (X.Qin, S.Hu, G.Zhou,
H.Zhang, J.Zhang, and S.Wang, Rare Metal Mater Eng, 45 (2016) .240-243.) it is anti-using solid phase
Ying Fa, YAG crystalline ceramics is prepared for using MgO as sintering aid vacuum-sintering, and transmitance is 82% at its 1020nm.Document 2
(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.Adopt
It is that sintering aid is prepared for Yb with MgO:YAG crystalline ceramics, its transmitance only 80.6% at 1100nm；Although document 3
(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.) by improving the technology of preparing of document 4, should by vacuum-sintering combination HIP sintering technology
Transmitance is promoted to 83.5% at the 1100nm of ceramics, but still has away from theoretical transmission certain gap.
The Mg adjuvant system YAG base transparent ceramic generally existings that document above is reported the problems such as transmitance is relatively low, far
Not as good as the optical quality of YAG monocrystalline, it is impossible to meet Solid State Laser application demand, it is main reason is that relative to Si auxiliary agent bodies
System, Mg agent systems are more difficult to promote the densification of YAG crystalline ceramics, are unfavorable for being lifted the optical quality of crystalline ceramics.In addition, on
State document to make annealing treatment vacuum-sintering YAG crystalline ceramics, in order to eliminate the Lacking oxygen of vacuum-sintering generation,
So similarly cause the reduction of Ceramic optical quality.This is because while annealing process be conducive to eliminate vacuum-sintering caused by oxygen
Room, but remaining micro- stomata in ceramic body further spreads and merged, drop easily in annealing process due to high temperature action
Low optical quality.Moreover, adulterated for Mg auxiliary agents, because Mg Doped ions replace YAG matrix ions, due to charge compensation
Lacking oxygen is formed, and then capture electronically forms F+Colour center.During annealing, these colour centers easily merge to be formed with Mg ions
[Mg2+F+] colour center, expand light abstraction width, further reduction Ceramic optical quality.
On the other hand, sintering aid is as a kind of " additional impurity ", if its adding too much, and the optics for being unfavorable for ceramics is equal
Even property, aggravates optical scattering.Therefore, on the premise of YAG crystalline ceramics good optical qualities are ensured, the addition of sintering aid
It is more few better.Although document 4 (A.Ikesue, Y.L.Aung, J.Klimke, J.Am.Ceram.Soc.100 (2017) 26-30.)
High-quality Yb is prepared in the case of without any sintering aid:YAG crystalline ceramics, and successfully realize that laser is exported.But
Preparation method is used for vacuum-sintering combination HIP sintering method.Although relative to vacuum-sintering, HIP sintering technology
Extra densification driving force can be provided for ceramic post sintering by impressed pressure, but HIP sintering is relative to true
Sky sintering, its high-pressure sinter environment is very high to equipment requirement, is unfavorable for saving the energy, and with certain risk.
Therefore, if under non-annealing mechanism, realized using the single auxiliary agent agent of a small amount of Mg under non-annealing mechanism high-quality
The preparation of YAG crystalline ceramics, then it will be that the refinement of YAG crystalline ceramics crystallite dimensions and the lifting of optical quality are provided effectively
With reference to.But so far, this area is not yet developed uses the single adjuvant systems of a small amount of Mg directly to exist under non-annealing mechanism
YAG transparent ceramic materials with good optical qualities and fine grain and preparation method thereof are prepared under vacuum condition.
Therefore, this area can meet Solid State Laser application demand in the urgent need to developing one kind under non-annealing mechanism,
The YAG bases with good optical qualities and fine grain distribution to be prepared under the single auxiliary agents of a small amount of Mg of the effectively save energy of energy transparent again
The method of ceramic material.
The content of the invention:
For it is existing the problem of, the present invention is provided under a kind of non-annealing mechanism, based on the mono- auxiliary agent vacuum-sintering systems of a small amount of Mg
Standby yttrium-aluminium-garnet (Y3Al5O12, YAG) crystalline ceramics method, so as to solve the problem of prior art is present.
The present invention is realized by following technical solution：
The present invention provides a kind of method for preparing YAG crystalline ceramics, and this method is under non-annealing mechanism, using Mg as single fire knot
Auxiliary agent, using single step vaccum sintering process prepare YAG crystalline ceramics, prepared crystalline ceramics component should meet following (1) formula or
Person (2) formula:
(RexY1-x)3Al5O12 (1)
Y3(CryAl1-y)5O12 (2)
X span is that 0≤x≤0.6, y scope is that 0≤y≤0.002, Re is Ce, Nd, Yb, Er, Ho in formula,
Dy, Pr, Tm, Sm, Eu or Tb one kind；Mg addition be Y, Al, Cr or Y, Al, Re raw material silty amount summation 0.005~
0.018wt.%.
Further, above-mentioned preparation method comprises the following steps：
Step one, raw material is chosen：Y of the Y raw materials from commercially available purity 99.99% and the above2O3Powder, Al raw materials select city
Sell the α-Al of purity 99.99% and the above2O3Powder, Re of the Re raw materials from commercially available purity 99.99% and the above2O3Powder or
ReO2Powder, Cr of the Cr raw materials from commercially available purity 99.99% and the above2O3Powder；Above-mentioned raw materials powder is pressed into required metal
After the stoichiometric proportion of element is weighed, it is placed in ball grinder, and adds Mg auxiliary agents, dispersant and absolute ethyl alcohol configuration slurry.
Step 2, ball milling and powder handling：The slurry that step one is configured is placed in 6~25h of ball milling in ball mill and obtains second
Alcohol based sizing；Above-mentioned slurry is placed in baking oven to be dried 5-48 hours at 30~150 DEG C, and dried slurry is ground
Sieve.
Step 3：Powder is molded：Powder after being sieved in step 2 is placed in mould, pressed using 10Mpa~100Mpa
Power is molded powder；Biscuit after shaping is placed in hermetic bag, in cold isostatic compaction under 80Mpa~350Mpa pressure；Will be upper
State the biscuit after isostatic cool pressing compacting to be placed in Muffle furnace, using 300~1100 DEG C of 2~15h of calcining, be then cooled to 30~50
℃。
Step 4：Biscuit is sintered：Biscuit of ceramics after the calcining that step 3 is obtained is placed in vacuum sintering furnace, is used
1680 DEG C~1860 DEG C 2~80h of vacuum-sintering, are then cooled to 30~50 DEG C；YAG ceramics after sintering are machined
Processing, obtains the YAG base transparent ceramic materials that thickness is 1~5mm.
Further, the present invention prepared by YAG transparent ceramic materials 1064nm at line transmitance be higher than 84.0%~
84.5%, thickness is 1~5mm；Ceramic crystalline grain size is 2.0~40 μm, and particle diameter distribution is uniform.
Further, ball grinder is high purity aluminium oxide ball grinder or nylon ball grinder in above-mentioned steps one；Mg raw materials are city
Sell high-purity (more than 99.99%) MgO, MgCO3,MgF2With Mg (OH)2One or more；The dispersant is DS005, and it adds
Dosage is 0.03~1.5wt% of Y, Al raw material silty amount summation；Final configuration slurry solid content is 20%~60%.
Further, the ball milling method in above-mentioned steps two is planetary ball mill or horizontal ball milling, and abrading-ball uses high pure zirconia
One kind of aluminium ball, high-purity zirconia ball or agate ball, drum's speed of rotation is 100~300r/min；Dried powder sieving 1~
8 times, screen number is 50~200 mesh.
Further, the mould used in above-mentioned steps three for rubber mold or stainless steel mould, cold isostatic compaction
Dwell time is 1~30min；Biscuit calcining heating rate is 0.5-20 DEG C/min, and rate of temperature fall is 3~30 DEG C/min, calcining
Atmosphere is air atmosphere or oxygen atmosphere.
Further, the sintering vacuum of above-mentioned steps four is higher than 10-3Pa, sintering heating rate is 0.5-10 DEG C/min,
Rate of temperature fall is 1~50 DEG C/min；The machining includes frosted and is thinned and polishing.
Detailed description of the invention
One the invention provides a kind under non-annealing mechanism, using vacuum-sintering system under the single adjuvant systems of a small amount of Mg
Standby yttrium-aluminium-garnet (Y3Al5O12, YAG) base transparent ceramic method, it is characterised in that using a small amount of Mg as single sintering aid, use
Single step vaccum sintering process, in the case where being not added with making annealing treatment with the later stage, prepares the transparent potteries of YAG with good optical qualities
Porcelain, prepared crystalline ceramics component should meet following (1) formula or (2) formula:
(RexY1-x)3Al5O12 (1)
Y3(CryAl1-y)5O12 (2)
X span is that 0≤x≤0.6, y scope is that 0≤y≤0.05, Re is Ce, Nd, Yb, Er, Ho, Dy in formula,
Pr, Tm, Sm, Eu or Tb one kind.Mg addition be Y, Al, Cr or Y, Al, Re raw material silty amount summation 0.003~
0.018wt.%.Line transmitance 84.0~84.5% at the YAG crystalline ceramics 1064nm finally prepared (1~5mm is thick).Crystal grain chi
Very little is 2.0~40 μm, and particle diameter distribution is uniform.
Comprise the following steps that：
Step one, raw material is chosen：Y raw materials are from commercially available high-purity (99.99% and more than) Y2O3Powder, Al raw materials select city
Sell high-purity (99.99% and more than) α-Al2O3Powder, Re raw materials are from commercially available high-purity (99.99% and more than) Re2O3Powder or
ReO2Powder, Cr raw materials are from commercially available high-purity (99.99% and more than) Cr2O3Powder.Above-mentioned raw materials powder is pressed into required metal
After the stoichiometric proportion of element is weighed, it is placed in ball grinder, and adds Mg auxiliary agents, dispersant and absolute ethyl alcohol configuration slurry.
Step 2, ball milling and powder handling：The slurry that step one is configured is placed in 6~25h of ball milling in ball mill and obtains second
Alcohol based sizing.Above-mentioned slurry is placed in baking oven to be dried 5-48 hours at 30~150 DEG C, and dried slurry is ground
Sieve.
Step 3：Powder is molded：Powder after being sieved in step 2 is placed in mould, pressed using 10Mpa~100Mpa
Power is molded powder.Biscuit after shaping is placed in hermetic bag, in cold isostatic compaction under 80Mpa~350Mpa pressure.Will be upper
State the biscuit after isostatic cool pressing compacting to be placed in Muffle furnace, using 300~1100 DEG C of 2~15h of calcining, be then cooled to 30~50
℃。
Step 4：Biscuit is sintered：Biscuit of ceramics after the calcining that step 3 is obtained is placed in vacuum sintering furnace, is used
1680 DEG C~1860 DEG C 2~80h of vacuum-sintering, are then cooled to 30~50 DEG C.It is not subject to post annealed processing.After sintering
YAG ceramics carry out machining processes, obtain the YAG base transparent ceramic materials that thickness is 1~5mm.
Further, ball grinder is high purity aluminium oxide ball grinder or nylon ball grinder in step one；Mg raw materials are commercially available height
Pure (more than 99.99%) MgO, MgCO3,MgF2With Mg (OH)2One or more；Wherein Mg elements addition be Y, Al, Cr or
0.003~0.018wt.% of Y, Al, Re raw material silty amount summation；The dispersant is DS005, and its addition is Y, Al raw material
0.03~1.5wt% of silty amount summation.Final configuration slurry solid content is 20%~60%.
Further, ball milling method is planetary ball mill or horizontal ball milling in step 2, and abrading-ball uses high purity aluminium oxide ball, high
One kind of pure zirconia ball or agate ball, drum's speed of rotation is 100~300r/min；Dried powder sieves 1~8 time, sieve
Hole mesh number is 50~200 mesh.
Further, the mould used in step 3 is rubber mold or stainless steel mould, the pressurize of cold isostatic compaction
Time is 1~30min；Biscuit calcining heating rate is 0.5-20 DEG C/min, and rate of temperature fall is 3~30 DEG C/min, calcination atmosphere
For air atmosphere or oxygen atmosphere.
Further, step 4 sintering vacuum is higher than 10-3Pa, sintering heating rate is 0.5-10 DEG C/min, cooling speed
Rate is 1~50 DEG C/min, and the machining includes frosted and is thinned and polishing.
Beneficial effect
The preparation method of the present invention, under non-annealing mechanism, can effectively suppress the diffusion of remaining micro- stomata with merging,
The ceramic scattering loss of reduction.Mg doping can promote YAG crystalline ceramics in relatively low sintering temperature (being less than 1660 DEG C)
Densification, and grain growth can be promoted between 1540 DEG C and 1660 DEG C of sintering temperature.Under relatively low densification temperature, energy
Enough densification temperatures that effectively expands are interval, and the ceramic sintering of promotion and densification are conducive to further excluding scattering center, tied
Non-annealing mechanism is closed, scattering loss can be effectively reduced, consistency height, the YAG crystalline ceramics of excellent in optical properties is obtained.Separately
Outside, Mg ions are mixed in YAG matrix, due to Mg2+Ionic radius and YAG lattices in hexa-coordinate Al3+Ionic radius is close,
With higher solid solubility, therefore it can lift diffusion coefficient effectively by vacancy mechanism, be conducive to ceramics sintered
The exclusion of stomata in journey, lifts its optical quality, reduces scattering loss.In addition, Mg with its+2 valence property, may advantageously facilitate one
High-valence state conversion (such as Cr of a little specific foreign atoms3+→Cr4+,Yb2+→Yb3+)。
Based on it is above-mentioned the characteristics of, summarize the present invention advantage it is as follows：
(1) present invention is under non-annealing mechanism, and realizing the single auxiliary agent vacuum-sinterings of a small amount of Mg, to prepare high-quality YAG bases saturating
Bright ceramics, while high-quality YAG crystalline ceramics is prepared, effectively reduce sintering aid addition.Prepared ceramics
Consistency is high, uniformity is good, segregation-free, without transgranular and intergranular stomata, and transmitance is high, meets the bar as gain medium
Part.
(2) present invention prepares the single adjuvant system YAG crystalline ceramics of a small amount of Mg using vaccum sintering process, without atmosphere auxiliary
With expensive pressure sintering equipment, simply, economical and energy saving effect is obvious for equipment.
(3) to realize YAG crystalline ceramics microstructural controllable by the present invention, and grade is with being reasonably distributed, and crystal grain without exception is long
Greatly, the easy segregation problems of Ca adjuvant systems are efficiently solved.Mg auxiliary agents advantageously reduce ceramics by its room flooding mechanism simultaneously
Scattering loss.
(4) this method technique is simple, it is not necessary to expensive high-tension apparatus, and its ceramic average grain size prepared is 2.0
~40 μm, particle diameter distribution is uniform, and excellent in optical properties, its 1064nm transmitance can reach 84.5%, can be used as Solid State Laser
The gain media of device；, short preparation period advantageously reduces cost requirement, realizes Technique Popularizing and business promotion.
Brief description of the drawings:
Fig. 1：According to embodiment 1, the XRD spectrum of the YAG base transparent ceramics described in 2,3,4 is pure YAG phases；
Fig. 2：The photo in kind for the YAG base transparent ceramics stated according to embodiment 2,3, illustrates that ceramics have good translucency
Can, excellent in optical properties.
Fig. 3：According to embodiment 2, the YAG base transparent ceramics polishing section SEM figures described in 4 show that the ceramics have complete
Densified structure
Fig. 4：According to the light microscope bright field image of the YAG base transparent ceramics described in embodiment 2, illustrate that the ceramics have
Good optical homogeneity.
Fig. 5：According to embodiment 2, the YAG base transparent ceramics surface SEM spectrum described in 4 shows that the ceramic crystalline grain size is equal
Even, no Residual Pores are present, excellent in optical properties.
Fig. 6：According to embodiment 2, the line transmittance curve of the YAG base transparent ceramics described in 3 shows that the ceramics have higher
Optical quality.
Embodiment 1,
1. by commercial concentration be 99.99% Y2O3, 99.99% Al2O3With 99.99% CeO2By (Ce0.01Y0.99)3Al5O12After stoichiometric proportion is weighed, it is placed in nylon ball grinder, is subsequently added the Mg (OH) that purity is 99.99%2Helped for sintering
Agent (wherein Mg mass percents be Y, Al, Ce material powder quality summation 0.003wt.%), 1wt%DS005 is as scattered
Agent, adds absolute ethyl alcohol and is configured to the slurry that solid content is 60%.
2. by step 1. in obtained slurry be placed on horizontal ball mill using high-purity zirconia ball ball milling mixing 6 hours,
Rotating speed is that the slurry after 300r/min, ball milling is placed at 150 DEG C dry 5h, and dried presoma is sieved, using 50 mesh
Mesh screen sieves 8 times.
3. by step, 2. resulting sieving powder is placed in rubber mold, is pressed into disk using 10Mpa dry-pressing, then pass through
Cross 350MPa isostatic cool pressings and biscuit is made, the dwell time is 1min.Biscuit is in air atmosphere using 1100 DEG C of calcinings, insulation 2
Hour, and it is cooled to 30 DEG C.Calcining heating rate is 20 DEG C/min, 30 DEG C/min of rate of temperature fall.
3. the biscuit after step 3. resulting calcining is placed in vacuum sintering furnace, using 1680 DEG C of vacuum-sintering 80h,
Vacuum is 10-3Pa, is then cooled to 30 DEG C.0.5 DEG C/min of heating rate, 1 DEG C/min of rate of temperature fall are sintered, densification is obtained
YAG crystalline ceramics, is not subject to post annealed processing.And frosted, to be polished to 1mm thick.XRD spectrum (the Bruker of ceramics sample
D2) see Fig. 1, be pure YAG phases.2 μm of crystallite dimension, transmitance is 84.0%, excellent in optical properties at 1064nm.
Embodiment 2,
1. by commercial concentration be 99.999% Y2O3, 99.999% Al2O3By Y3Al5O12After stoichiometric proportion is weighed,
It is placed in ceramic ball grinder, it is that (wherein Mg mass percents are Y, Al to sintering aid to be subsequently added the MgO that purity is 99.999%
The 0.018wt.% of material powder quality summation).Using 0.03wt%DS005 as dispersant, add absolute ethyl alcohol and be configured to
Solid content is 30% slurry.
2. by step 1. in obtained slurry be placed on planetary ball mill it is small using high purity aluminium oxide ball ball milling mixing 12
When, rotating speed is that the slurry after 200r/min, ball milling is placed at 50 DEG C dry 30h, and dried presoma is sieved, and is used
100 mesh mesh screens sieve 4 times.
3. by step, 2. resulting sieving powder is placed in stainless steel mould, and disk is pressed into using 20Mpa dry-pressing, then
Biscuit is made by 200MPa isostatic cool pressings, the dwell time is 10min.Biscuit is in air atmosphere using 800 DEG C of calcinings, insulation
4 hours, and it is cooled to 30 DEG C.Calcining heating rate is 2 DEG C/min, 3 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 10-5Pa, is then cooled to 30 DEG C.2 DEG C/min of heating rate, 5 DEG C/min of rate of temperature fall are sintered, densification is obtained
YAG crystalline ceramics, is not subject to post annealed processing.And frosted, to be polished to 3mm thick.The XRD spectrum of ceramics sample is shown in Fig. 1, is
Pure YAG phases；Sample transmitance collection of illustrative plates (Lambda 950) as shown in fig. 6, its at 1064nm line transmitance be 84.5%, show
Sample has good optical quality；The surface of sample and section SEM spectrum are shown in Fig. 2 and Fig. 3 respectively, show that the ceramics have had
Full densification microstructure, pore-free and intergranular are mutually present, and crystallite dimension is 22 μm；.Sample light microscope (Axio
Scope.A1) collection of illustrative plates is shown in Fig. 4, and no scattering center is present, excellent in optical properties.
Embodiment 3,
1. by commercial concentration be 99.99% Y2O3, 99.999% Al2O3With 99.99% Cr2O3Press
(Cr0.002Y0.998)3Al5O12After stoichiometric proportion is weighed, it is placed in ceramic ball grinder, it is 99.99% to be subsequently added purity
MgCO3For sintering aid (wherein Mg mass percents be Y, Al, Cr material powder quality summation 0.012wt.%),
0.2wt%DS005 adds absolute ethyl alcohol and is configured to the slurry that solid content is 40% as dispersant.
2. by step 1. in obtained slurry be placed on planetary ball mill using aluminum oxide ball milling mixing 18 hours, rotating speed
For 180r/min, the slurry after ball milling, which is placed at 110 DEG C, dries 10h, and dried presoma is sieved, using 150 mesh nets
It is sieved through sieve 3 times.
3. by step, 2. resulting sieving powder is placed in stainless steel mould, and disk is pressed into using 100Mpa dry-pressing,
Biscuit is made by 280MPa isostatic cool pressings again, the dwell time is 5min.Biscuit, using 500 DEG C of calcinings, is protected in air atmosphere
Temperature 10 hours, and it is cooled to 40 DEG C.Calcining heating rate is 5 DEG C/min, 15 DEG C/min of rate of temperature fall.
3. the biscuit after step 3. resulting calcining is placed in vacuum sintering furnace, using 1740 DEG C of vacuum-sintering 50h,
Vacuum is 10-5Pa, is then cooled to 40 DEG C.0.5 DEG C/min of heating rate, 25 DEG C/min of rate of temperature fall are sintered, densification is obtained
YAG crystalline ceramics, be not subject to post annealed processing.And frosted, to be polished to 3mm thick.The XRD spectrum of ceramics sample is shown in Fig. 1,
For pure YAG phases；The polished surface collection of illustrative plates of sample is shown in Fig. 2, shows that the ceramics have a complete densification microstructure, pore-free and
Intergranular is mutually present, and crystallite dimension is tiny, and crystallite dimension is 40 μm, and sample transmitance is shown in Fig. 6, and transmitance is at its 1064nm
84.5%, excellent in optical properties.
Embodiment 4,
1. by commercial concentration be 99.99% Y2O3, 99.99% Al2O3With 99.999 Yb2O3By (Yb0.6Y0.4)3Al5O12After stoichiometric proportion is weighed, it is placed in ceramic ball grinder, is subsequently added the MgF that purity is 99.99%2For sintering aid
(wherein Mg mass percents be Y, Al material powder quality summation 0.01wt%).Using 1.5wt%DS005 as scattered
Agent, adds absolute ethyl alcohol and is configured to the slurry that solid content is 20%.
2. by step 1. in obtained slurry be placed on planetary ball mill using high-purity agate ball milling mixing 25 hours, turn
Speed is that the slurry after 100r/min, ball milling is placed at 30 DEG C dry 48h, and dried presoma is sieved, using 200 mesh nets
It is sieved through sieve 1 time.
3. by step, 2. resulting sieving powder is placed in stainless steel mould, and disk is pressed into using 100Mpa dry-pressing,
Biscuit is made by 80MPa isostatic cool pressings again, the dwell time is 30min.Biscuit, using 300 DEG C of calcinings, is protected in oxygen atmosphere
Temperature 15 hours, and it is cooled to 50 DEG C.Calcining heating rate is 0.5 DEG C/min, 30 DEG C/min of rate of temperature fall.
4. the biscuit after step 3. resulting calcining is placed in vacuum sintering furnace, using 1860 DEG C of vacuum-sintering 2h,
Vacuum is 10-4Pa, is then cooled to 50 DEG C.10 DEG C/min of heating rate, 50 DEG C/min of rate of temperature fall are sintered, densification is obtained
YAG crystalline ceramics, is not subject to post annealed processing.And frosted, to be polished to 5mm thick.The XRD spectrum of ceramics sample is shown in Fig. 1, is
Pure YAG phases；Line transmitance is 84.2% at its 1064nm, close to YAG theoretical transmissions, the section and surface SEM spectrum of sample
Fig. 3 and Fig. 5 are seen respectively, show that the ceramics have complete densification microstructure, pore-free and intergranular are mutually present, crystallite dimension
For 28 μm；Show the excellent in optical properties of sample.
Claims (7)
1. a kind of method for preparing YAG crystalline ceramics, it is characterised in that under non-annealing mechanism, using Mg as single sintering aid, is adopted
YAG crystalline ceramics is prepared with single step vaccum sintering process, prepared crystalline ceramics component should meet following (1) formula or (2) formula:
(RexY1-x)3Al5O12 (1)
Y3(CryAl1-y)5O12 (2)
X span is that 0≤x≤0.6, y scope is that 0≤y≤0.002, Re is Ce, Nd, Yb, Er, Ho, Dy, Pr in formula,
Tm, Sm, Eu or Tb one kind；Mg addition be Y, Al, Cr or Y, Al, Re raw material silty amount summation 0.005~
0.018wt.%.
2. the method for preparing YAG crystalline ceramics according to right 1, it is characterised in that described preparation method step is as follows：
Step one, raw material is chosen：Y of the Y raw materials from commercially available purity 99.99% and the above2O3Powder, Al raw materials are from commercially available pure
α-the Al of degree 99.99% and the above2O3Powder, Re of the Re raw materials from commercially available purity 99.99% and the above2O3Powder or ReO2Powder
Body, Cr of the Cr raw materials from commercially available purity 99.99% and the above2O3Powder；By above-mentioned raw materials powder by required metallic element
After stoichiometric proportion is weighed, it is placed in ball grinder, and adds Mg auxiliary agents, dispersant and absolute ethyl alcohol configuration slurry.
Step 2, ball milling and powder handling：The slurry that step one is configured is placed in 6~25h of ball milling in ball mill and obtains ethanol base
Slurry；Above-mentioned slurry is placed in baking oven to be dried 5-48 hours at 30~150 DEG C, and dried slurry is ground into sieving.
Step 3：Powder is molded：Powder after being sieved in step 2 is placed in mould, made using 10Mpa~100Mpa pressure
Powder is molded；Biscuit after shaping is placed in hermetic bag, in cold isostatic compaction under 80Mpa~350Mpa pressure；Will be above-mentioned cold
Biscuit after isostatic pressed compacting is placed in Muffle furnace, using 300~1100 DEG C of 2~15h of calcining, is then cooled to 30~50 DEG C.
Step 4：Biscuit is sintered：Biscuit of ceramics after the calcining that step 3 is obtained is placed in vacuum sintering furnace, using 1680 DEG C
~1860 DEG C of 2~80h of vacuum-sintering, are then cooled to 30~50 DEG C；YAG ceramics after sintering carry out machining processes,
Obtain thickness YAG base transparent ceramic materials.
3. the method according to claim 1 or 2 for preparing YAG crystalline ceramics, it is characterised in that the YAG of described preparation
Transparent ceramic material line transmitance at 1064nm is higher than 84.0%~84.5%, and thickness is 1~5mm；Ceramic crystalline grain size is
2.0~40 μm, particle diameter distribution is uniform.
4. the described method for preparing YAG crystalline ceramics according to claim 2, it is characterised in that ball milling in step one
Tank is high purity aluminium oxide ball grinder or nylon ball grinder；Mg raw materials are commercially available high-purity (more than 99.99%) MgO, MgCO3,MgF2With
Mg(OH)2One or more；The dispersant be DS005, its addition for Y, Al raw material silty amount summation 0.03~
1.5wt%；Final configuration slurry solid content is 20%~60%.
5. the described method for preparing YAG crystalline ceramics according to claim 2, it is characterised in that ball milling in step 2
Mode is planetary ball mill or horizontal ball milling, and abrading-ball uses one kind of high purity aluminium oxide ball, high-purity zirconia ball or agate ball, ball milling
Machine rotating speed is 100~300r/min；Dried powder sieves 1~8 time, and screen number is 50~200 mesh.
6. the described method for preparing YAG crystalline ceramics according to claim 2, it is characterised in that used in step 3
Mould be rubber mold or stainless steel mould, dwell time of cold isostatic compaction is 1~30min；Biscuit calcining heating speed
Rate is 0.5-20 DEG C/min, and rate of temperature fall is 3~30 DEG C/min, and calcination atmosphere is air atmosphere or oxygen atmosphere.
7. the described method for preparing YAG crystalline ceramics according to claim 2, it is characterised in that step 4 sintering is true
Reciprocal of duty cycle is higher than 10-3Pa, sintering heating rate is 0.5-10 DEG C/min, and rate of temperature fall is 1~50 DEG C/min；The machining bag
Frosted is included to be thinned and polishing.
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