CN102249679A - Method for preparing Ho<3+> doped yttrium lanthanum oxide transparent ceramic material - Google Patents

Method for preparing Ho<3+> doped yttrium lanthanum oxide transparent ceramic material Download PDF

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Publication number
CN102249679A
CN102249679A CN201110154167XA CN201110154167A CN102249679A CN 102249679 A CN102249679 A CN 102249679A CN 201110154167X A CN201110154167X A CN 201110154167XA CN 201110154167 A CN201110154167 A CN 201110154167A CN 102249679 A CN102249679 A CN 102249679A
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powder
ceramic material
ball milling
oxide transparent
sintering
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黄栋栋
杨秋红
张浩佳
陆神洲
王永刚
李韫含
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a Ho<3+> doped yttrium lanthanum oxide transparent ceramic material applicable to the light emission of an intermediate infrared waveband (2 mu m), and a preparation method thereof and belongs to the field of special ceramic material manufacturing processes. The ceramic material provided by the invention is characterized in that domestic high-purity Ho2O3 nano-powder, La2O3 nano-powder and Y2O3 nano-powder are taken as raw materials; an appropriate sintering system is formulated by adopting a traditional ceramic preparation process; and finally, the Ho<3+> doped yttrium lanthanum oxide transparent ceramic material is prepared by adopting a solid-state sintering method under the condition of lower temperature. Through test determination, the ceramic material has a wider emitting band near a 2 mu m waveband, which shows that the Ho<3+> doped yttrium lanthanum oxide transparent ceramic material is expected to be a 2 mu m laser working medium material.

Description

Mix Ho＜sup〉3+＜/sup〉preparation method of lanthanum yttrium oxide transparent stupalith
Technical field
The present invention relates to mix Ho 3+Lanthanum yttrium oxide transparent stupalith and preparation method thereof belongs to the special cermacis manufacturing process technology field.
Background technology
2 mu m wavebands are positioned at an absorption peak of water, atmospheric window wave band and safety range of human eye, therefore 2 μ m laser have important use, the pumping source of infrared 3 ~ 5 μ m optical parametric oscillators (OPO) in can being used as in addition at aspects such as atmospheric remote sensing, optical communication, lidar and medical facilities.In all rare earth ions, Tm 3+Ionic 3F 4→ 3H 6Energy level transition and Ho 3+Ionic 5I 7→ 5I 8Energy level transition is to obtain 2 mu m luminous main paties.Ho 3+Ion has abundant energy level, big stimulated emission cross section and the fluorescence lifetime of growing (8ms), is the 2 μ m laser active ions that have development potentiality most.1962, people such as the Johnson of the U.S. were mixing Ho 3+Ionic CaWO 4Obtained the laser output of 2.09 μ m in the crystal first, but because high threshold energy and working at low temperatures there is not actual application value.Research at present laserable material more widely mainly is rare earth ion doped crystal and glass material, and transparent ceramic material is because some advantages of self have also obtained research in the last few years.
Laser transparent ceramic has a lot of monocrystalline and the not available advantage of glass: compare with monocrystalline, crystalline ceramics has the doping content height, uniform doping is good, sintering temperature is low, cycle is short, and cost is low, and quality controllability is strong, size is big, and freedom shape is big and can realize advantage such as multi-layer multi laser apparatus; With the glassy phase ratio, it is good that crystalline ceramics has monochromaticity, and structure is formed even more ideal, thermal conductivity height and the radiation power advantages of higher that can bear.Because pottery is a polycrystalline, the imperfection of its inner crystal boundary, pore, lattice etc. all can cause the opacity of material and increase the scattering of light loss, therefore uses it for laser medium and has certain difficulty.In order to prepare the laser ceramics of suitable with the monocrystalline laser activity high-quality, high-clarity, people have done a large amount of research work.
Y 2O 3Be to study more a kind of laser host material at present, yttrium oxide belongs to isometric system, the free of birefringence phenomenon, and the thermal conductivity height is that the twice of YAG is many, Y 2O 3Crystal is a kind of good Solid State Laser substrate material.But because Y 2O 3Fusing point up to 2430 ℃, and near 2280 ℃ cube polycrystalline phase transformation of six side's phases in opposite directions can take place, thereby be difficult to grow the Y of large size and high optical quality 2O 3Monocrystalline.Along with the development of ceramics processing and nanometer powder-making technique, Y 2O 3The sintering temperature of crystalline ceramics can be reduced to about 1700 ℃.By at Y 2O 3Add La in the powder 2O 3Powder can quicken pore and get rid of, and promotes Y 2O 3Ceramic post sintering further reduces the sintering temperature of crystalline ceramics and effectively suppresses ceramic crystalline grain and too grow up, so the lanthanum yttrium oxide transparent pottery is a kind of laser host material of excellent property.
At present, crystal, glass and minority crystalline ceramics matrix have realized the laser output at 2 μ m places by doping with rare-earth ions.By with Ho 3+Ion doping utilizes Ho in the lanthanum yttrium oxide transparent ceramic substrate of excellent property 3+Ion exists 5I 7→ 5I 8Transition on the energy level, thus the laser output of 2 mum wavelengths obtained, mix Ho 3+The lanthanum yttrium oxide transparent pottery is expected to become a kind of 2 μ m laser working medium materials with development potentiality.
Summary of the invention
The objective of the invention is to adopt homemade high-purity Ho 2O 3, La 2O 3And Y 2O 3Nano powder is a raw material, adopts traditional ceramics preparation technology, formulates suitable sintering schedule, under lower temperature conditions, adopts the solid sintering technology preparation to mix Ho at last 3+The lanthanum yttrium oxide transparent stupalith.
A kind of Ho that mixes of the present invention 3+The preparation method of lanthanum yttrium oxide transparent stupalith is characterized in that it has following technological process and step:
A. adopt high-purity homemade 99.99% Ho 2O 3, 99.99% La 2O 3And 99.99%Y 2O 3Nano powder is a raw material, and three's mole proportioning is pressed chemical molecular formula Y 2-2x-2yLa 2xHo 2yO 3, the x=0.01 in the formula～0.20, y=0.005 ~ 0.10;
B. the Y that will prepare by said ratio 2-2x-2yLa 2xHo 2yO 3Mixed powder is put into ball grinder and is carried out ball milling, mixed powder ball milling 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
C. ball milling is good powder is calcined powder mix then in drying in oven in retort furnace, 1200 ℃ are incubated 10 hours, and naturally cooling obtains Ho:Y 2-2xLa2xO3 (Be Y 2-2x-2yLa 2xHo 2yO 3) powder;
D. once more powder is put into the spheroidal graphite jar and carried out ball milling, ball milling is 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
E. ball milling is good powder carries out granulation in drying in oven with powder, crosses 40 mesh sieves;
F. the powder after the granulation is dry-pressing formed, depress to the sheet sample in the 200MPa isostatic cool pressing subsequently;
G. said sample is placed in the molybdenum wire furnace, under the normal pressure reducing atmosphere, carries out sintering; Sintering range is 1500～1700 ℃, and sintering time is 40 ~ 45 hours, the final Ho:Y that obtains densification 2-2xLa2xO3 (Be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Description of drawings
Fig. 1 mixes Ho for the present invention 3+The emmission spectrum of lanthanum yttrium oxide transparent pottery.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
In the present embodiment, Ho is mixed in preparation 3+The concrete processing step of lanthanum yttrium oxide transparent pottery is as follows:
A. adopt high-purity homemade 99.99% Ho 2O 3, 99.99% La 2O 3And 99.99%Y 2O 3Nano powder is a raw material, and three's quality proportioning is pressed chemical molecular formula Y 2-2x-2yLa 2xHo 2yO 3, the x=0.10 in the formula, y=0.01; The molar content of each composition is: Ho 2O 30.01mol, La 2O 30.10mol, Y 2O 30.89mol;
B. by said ratio weighing Ho 2O 3, La 2O 3And Y 2O 3Powder is put into ball grinder and is carried out ball milling, compound ball milling 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
C. ball milling is good powder is put into baking oven, and oven dry is calcined powder mix in retort furnace at a certain temperature, 1200 ℃ of insulation 10h, naturally cooling;
D. once more powder is put into ball grinder and carry out ball milling, ball milling is 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
E. ball milling is good powder carries out granulation in drying in oven with powder, crosses 40 mesh sieves;
F. the powder after the granulation is dry-pressing formed, depress to the sheet sample in the 200MPa isostatic cool pressing subsequently;
G. said sample is placed in the molybdenum wire furnace, under the normal pressure reducing atmosphere, carries out sintering; Sintering temperature is 1580 ℃, and sintering time is 45 hours, the Ho that mixes that finally prepares densification and have favorable optical performance 3+The lanthanum yttrium oxide transparent pottery.
Embodiment 2
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.01 in the formula, y=0.02; The molar content of each composition is: Ho 2O 30.02mol, La 2O 30.01mol, Y 2O 30.97mol; 1630 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 3
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.01 in the formula, y=0.03; The molar content of each composition is: Ho 2O 30.03mol, La 2O 30.01mol, Y 2O 30.96mol; 1630 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 4
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.05 in the formula, y=0.05; The molar content of each composition is: Ho 2O 30.05mol, La 2O 30.05mol, Y 2O 30.90mol; 1580 ℃ of sintering temperatures, soaking time 40h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 5
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.05 in the formula, y=0.08; The molar content of each composition is: Ho 2O 30.08mol, La 2O 30.05mol, Y 2O 30.87mol; 1580 ℃ of sintering temperatures, soaking time 40h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 6
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.05 in the formula, y=0.10; The molar content of each composition is: Ho 2O 30.10mol, La 2O 30.05mol, Y 2O 30.85mol; 1580 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 7
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.075 in the formula, y=0.01; The molar content of each composition is: Ho 2O 30.01mol, La 2O 30.075mol, Y 2O 30.915mol; 1580 ℃ of sintering temperatures, soaking time 40h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 8
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.075 in the formula, y=0.02; The molar content of each composition is: Ho 2O 30.02mol, La 2O 30.075mol, Y 2O 30.905mol; 1580 ℃ of sintering temperatures, soaking time 40h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 9
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.10 in the formula, y=0.005; The molar content of each composition is: Ho 2O 30.005mol, La 2O 30.10mol, Y 2O 30.895mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 10
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.10 in the formula, y=0.03; The molar content of each composition is: Ho 2O 30.03mol, La 2O 30.10mol, Y 2O 30.87mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 11
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.10 in the formula, y=0.05; The molar content of each composition is: Ho 2O 30.05mol, La 2O 30.10mol, Y 2O 30.85mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 12
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.10 in the formula, y=0.08; The molar content of each composition is: Ho 2O 30.08mol, La 2O 30.10mol, Y 2O 30.82mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 13
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.10 in the formula, y=0.10; The molar content of each composition is: Ho 2O 30.10mol, La 2O 30.10mol, Y 2O 30.80mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 14
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.15 in the formula, y=0.01; The molar content of each composition is: Ho 2O 30.01mol, La 2O 30.15mol, Y 2O 30.84mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 15
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.15 in the formula, y=0.02; The molar content of each composition is: Ho 2O 30.02mol, La 2O 30.15mol, Y 2O 30.83mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 16
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.15 in the formula, y=0.05; The molar content of each composition is: Ho 2O 30.05mol, La 2O 30.15mol, Y 2O 30.80mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 17
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.20 in the formula, y=0.01; The molar content of each composition is: Ho 2O 30.01mol, La 2O 30.20mol, Y 2O 30.79mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 18
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.20 in the formula, y=0.05; The molar content of each composition is: Ho 2O 30.05mol, La 2O 30.20mol, Y 2O 30.75mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 19
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.20 in the formula, y=0.07; The molar content of each composition is: Ho 2O 30.07mol, La 2O 30.20mol, Y 2O 30.73mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
Embodiment 20
The processing step of present embodiment and the foregoing description 1 are identical, and that different is Y 2-2x-2yLa 2xHo 2yO 3X=0.20 in the formula, y=0.09; The molar content of each composition is: Ho 2O 30.09mol, La 2O 30.20mol, Y 2O 30.71mol; 1530 ℃ of sintering temperatures, soaking time 45h obtains fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
By above-mentioned examples preparation fine and close Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics, have the good optical performance.Material preparation process of the present invention is simple, and low cost of manufacture helps industrial scale production.(Trix-550, Jobin Yvon Spex France) detect the emmission spectrum of crystalline ceramics sample by fluorescence spectrum analyzer, as shown in Figure 1, can find to have near 2 μ m the emission band of a broad, the strongest emission peak is positioned at the 2018nm place, and Ho is mixed in this explanation 3+The lanthanum yttrium oxide transparent pottery is expected to become a kind of 2 μ m laser working medium materials.

Claims (1)

1. mix Ho for one kind 3+The preparation method of lanthanum yttrium oxide transparent stupalith is characterized in that it has following technological process and step:
Adopt high-purity homemade 99.99% Ho 2O 3, 99.99% La 2O 3And 99.99%Y 2O 3Nano powder is a raw material, and three's mole proportioning is pressed chemical molecular formula Y 2-2x-2yLa 2xHo 2yO 3, the x=0.01 in the formula～0.20, y=0.005 ~ 0.10;
The Y that will prepare by said ratio 2-2x-2yLa 2xHo 2yO 3Mixed powder is put into ball grinder and is carried out ball milling, mixed powder ball milling 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
The powder that ball milling is good is calcined powder mix then in drying in oven in retort furnace, 1200 ℃ are incubated 10 hours, and naturally cooling obtains Ho:Y 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) powder;
Once more powder is put into the spheroidal graphite jar and carried out ball milling, ball milling is 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
The powder that ball milling is good carries out granulation in drying in oven with powder, crosses 40 mesh sieves;
Powder after the granulation is dry-pressing formed, depress to the sheet sample in the 200MPa isostatic cool pressing subsequently;
Said sample is placed in the molybdenum wire furnace, under the normal pressure reducing atmosphere, carries out sintering; Sintering range is 1500～1700 ℃, and sintering time is 40 ~ 45 hours, the final Ho:Y that obtains densification 2-2xLa 2xO 3(be Y 2-2x-2yLa 2xHo 2yO 3) crystalline ceramics.
CN201110154167XA 2011-06-10 2011-06-10 Method for preparing Ho<3+> doped yttrium lanthanum oxide transparent ceramic material Pending CN102249679A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102659409A (en) * 2012-02-24 2012-09-12 上海大学 Preparation method for Ho<3+>-Yb<3+>-co-doped yttrium lanthanum oxide laser transparent ceramic material
CN102674839A (en) * 2012-05-23 2012-09-19 上海大学 Preparation method of Tm<3+>-doped yttrium lanthanum oxide laser transparent ceramic material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4147744A (en) * 1977-07-11 1979-04-03 Gte Laboratories Incorporated Transparent yttria ceramics and method for producing same
CN101148357A (en) * 2007-09-13 2008-03-26 上海大学 Method for preparing Yb3+ mixed lanthanum yttrium oxide upconversion luminous transparent laser ceramic
CN101148356A (en) * 2007-09-13 2008-03-26 上海大学 Ce3+ mixed lanthanum yttrium oxide transparent flickering ceramic material and preparation method thereof
WO2009063388A2 (en) * 2007-11-14 2009-05-22 Koninklijke Philips Electronics N.V. Green emitting solid-state laser comprising a sesquioxide and/or ceramic material
CN101665695A (en) * 2009-09-25 2010-03-10 上海大学 Preparation method of Pr<3+> doped (Yx La (1-x)) 2 O3 luminescent material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4147744A (en) * 1977-07-11 1979-04-03 Gte Laboratories Incorporated Transparent yttria ceramics and method for producing same
CN101148357A (en) * 2007-09-13 2008-03-26 上海大学 Method for preparing Yb3+ mixed lanthanum yttrium oxide upconversion luminous transparent laser ceramic
CN101148356A (en) * 2007-09-13 2008-03-26 上海大学 Ce3+ mixed lanthanum yttrium oxide transparent flickering ceramic material and preparation method thereof
WO2009063388A2 (en) * 2007-11-14 2009-05-22 Koninklijke Philips Electronics N.V. Green emitting solid-state laser comprising a sesquioxide and/or ceramic material
CN101665695A (en) * 2009-09-25 2010-03-10 上海大学 Preparation method of Pr<3+> doped (Yx La (1-x)) 2 O3 luminescent material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102659409A (en) * 2012-02-24 2012-09-12 上海大学 Preparation method for Ho<3+>-Yb<3+>-co-doped yttrium lanthanum oxide laser transparent ceramic material
CN102674839A (en) * 2012-05-23 2012-09-19 上海大学 Preparation method of Tm<3+>-doped yttrium lanthanum oxide laser transparent ceramic material

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Application publication date: 20111123