CN102320834B - Yb<3+>-doped (ScxY1-x)2O3 laser transparent ceramic applicable to femtosecond pulse laser and preparation method thereof - Google Patents

Yb<3+>-doped (ScxY1-x)2O3 laser transparent ceramic applicable to femtosecond pulse laser and preparation method thereof Download PDF

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CN102320834B
CN102320834B CN 201110154903 CN201110154903A CN102320834B CN 102320834 B CN102320834 B CN 102320834B CN 201110154903 CN201110154903 CN 201110154903 CN 201110154903 A CN201110154903 A CN 201110154903A CN 102320834 B CN102320834 B CN 102320834B
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CN102320834A (en
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陆神洲
杨秋红
史治法
黄栋栋
王永刚
李韫含
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University of Shanghai for Science and Technology
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Abstract

The invention relates to Yb<3+>-doped (ScxY1-x)2O3 laser transparent ceramic applicable to a femtosecond pulse laser and a preparation method thereof, belonging to the technical field of manufacturing of special ceramic materials. The method is characterized in that: the Yb<3+>-doped (ScxY1-x)2O3 laser transparent ceramic is prepared from high-purity Yb2O3, Y2O3 and Sc2O3 nano powder serving as raw materials by adopting a solid phase sintering method under the condition of low temperature. As proved by a detection experiment, the Yb<3+>-doped (ScxY1-x)2O3 laser transparent ceramic prepared with the method has a wide emitting bandwidth, and can be used for realizing femtosecond-grade ultrafast pulse laser output.

Description

A kind of Yb that can be used for femtosecond pulse laser 3+(Sc mixes xY 1-x) 2O 3Crystalline ceramics and preparation method thereof
Technical field
The present invention relates to a kind of Yb that can be used for femtosecond pulse laser 3+(Sc mixes xY 1-x) 2O 3Laser transparent ceramic and preparation method thereof belongs to the special cermacis manufacturing process technology field.
Background technology
Various ultrafast dynamic processes provide powerful instrument to the femtosecond laser technology that develop rapidly the nineties in last century for people study.Occurring in nature exists the temporal resolution restriction that is subjected to measurement means before many and the ultrafast phenomenas that can't be familiar with, all occurs in femtosecond to the scope of psec as the fracture of the motion on the molecular scale, chemical bond and formation etc.Mode-locking technique makes laser pulse width shorten to the order of magnitude of femtosecond quickly, provides time-resolved possibility for studying these ultrafast phenomenas, and therefore the research range of many traditional subjects has obtained great expansion, and the new natural law is anxious to be waited to find.Nobel chemistry Prize had just been authorized U.S. scientist Ahmed Zewail in 1999, to commend him in the development work aspect the femtochemistry.Femto-second laser has been widely used in fields such as ultrafast spectroscopy, microelectronics processing, biologic medical, metering, holographic imaging, heavy body and high-speed light communication at present.Can believe that along with the development of femtosecond laser technology, it will play an increasingly important role, for new contribution is made in the developing of natural science technology and high technology industry in the development of physics, biology, chemistry and other related disciplines.
The progress of laserable material is an important ring that influences the femto-second laser development.Up to now, titanium jewel (Ti:Al 2O 3) be still the ultra-short pulse laser material of output performance the best.Yet the quantum loss of titanium jewel is big, when high power pump, can produce a large amount of heats, thus to cooling system require highly, and used pumping source equipment is big and expensive, these have all restricted the commercial applications of titanium jewel femto-second laser, so people have invested more sight and mix Yb 3+Laserable material.With Nd 3+Wait other rare earth ion to compare Yb 3+The ion level structure is simple, does not have excited state absorption and cross-relation effect, and quantum loss is low, and fluorescence lifetime length (is Nd approximately 3+3 times of same material), energy storage capacity is strong.The emission band at its 1 μ m place has remedied the disappearance of titanium jewel emmission spectrum at this wave band place, industrial special purpose is arranged.Particularly noticeable is to mix Yb 3+Laser medium generally has wideer absorption and emission band, is conducive to laser diode (LD) pumping and produces ultrashort pulse.In this case, carry out and mix Yb 3+The research of all solid state laser becomes the focus of Development of New Generation compact type, high-level efficiency, low-cost femto-second laser.
Cube phase sesquioxide Ln 2O 3(Ln=Y Sc) is realizing having its unique advantage aspect the femtosecond pulse.Their chemistry, optics and mechanical property excellence, and the very high (Y of thermal conductivity 2O 3=13.6 W/mK, Sc 2O 3=16.5 W/mK), can effectively be suppressed at the thermal lensing effect that produces under the high power pump condition.Even to this day, Yb:Sc 2O 3And Yb:Y 2O 3All realized less than the output of the mode locking pulse of 100fs, in this case, shorter femtosecond, and even the generation of chirped pulse and be applied to fresh target into the people struggle.According to the locked mode principle, have only wide bandwidth of an emission could obtain ultrashort pulse width, therefore if can be at Yb:Sc 2O 3And Yb:Y 2O 3On the basis of excellent pulse laser performance, their bandwidth of an emission is carried out sufficient broadening, certainly will be able to make and mix Yb 3+The mode locking pulse laser activity of solid statelaser obtains corresponding raising.Because Yb:Sc 2O 3 2F 7/2The Stark splitting degree of energy level is greater than other Yb 3+Doping sesquioxide, so its emission peak positions and Yb:Y 2O 3, Yb:Lu 2O 3Differ 8 ~ 10nm.So pass through Yb:Sc 2O 3With other Yb 3+The doping sesquioxide is compound, can realize the stack of two kinds of material emission peaks, obtains wideer bandwidth of an emission.
Show Y according to phasor 2O 3With Sc 2O 3Can be by the arbitrary proportion solid solution, gained sosoloid Sc 2xY 2-2xO 3Still being a cube phase structure, not having birefringent phenomenon, is a kind of potential laser host material, can be used for preparing above-mentioned Yb 3+The doped and compounded sesquioxide is to realize Yb 3+The broadening of emission of ions bandwidth.Yet Y 2O 3And Sc 2O 3Fusing point very high (all being higher than 2400 ℃), and Y 2O 3Near 2280 ℃, also can take place by cube polycrystalline phase transformation of six side's phases in opposite directions, so will grow the Y of large size, high optical quality 2O 3-Sc 2O 3The system monocrystalline is very difficult.Along with the development of ceramics processing, the sintering temperature of rare-earth sesquioxide crystalline ceramics can be reduced to about 1700 ℃, the corresponding reduction of preparation cost.Compare monocrystalline, Yb:(Sc xY 1-x) 2O 3The crystalline ceramics preparation cost is low, Yb 3+Doping content height and good uniformity can be made large size and complex-shaped sample, suitable batch production.Show Yb:(Sc through the emmission spectrum test xY 1-x) 2O 3Each emission peak live width of crystalline ceramics is at Yb:Sc 2O 3And Yb:Y 2O 3The basis on broadening has largely all taken place, be more suitable for realizing the ultrashort mode locking pulse laser output of femtosecond.
Summary of the invention
The objective of the invention is to solve present Yb 3+The bandwidth of an emission of doping sesquioxide laserable material is wide inadequately, is not enough to obtain the problem of femtosecond ultra-short pulse laser output, and the spy provides a kind of wide Yb:(Sc of broad emission band that has xY 1-x) 2O 3Transparent laser is made pottery and preparation method thereof, to satisfy the ultra-short pulse laser research field for the wide Yb of broad emission band 3+The needs of doping solid laser material.This transparent ceramic material adopts high-purity Yb 2O 3, Y 2O 3And Sc 2O 3Be raw material, under lower temperature conditions, prepare with ceramic process.With Yb 3+The Y that mixes 2O 3And Sc 2O 3Monocrystalline is compared, and it has, and preparation technology is simple, with short production cycle, cost is low, is easy to characteristics such as large size preparation.Its wideer bandwidth of an emission is conducive to realize the mode locking pulse laser output of more lacking, the kind that has expanded this field solid laser material.
The present invention is a kind of Yb that can be used for the femtosecond pulse field 3+(Sc mixes xY 1-x) 2O 3The preparation method of transparent laser ceramic is characterized in that having following technological process and step:
A. adopt high-purity Yb 2O 3(99.99%), Y 2O 3(99.99%) and Sc 2O 3(99.99%) nano powder is raw material, with Y 2O 3And Sc 2O 3Be body material, Yb 2O 3Be dopant material.Three's mole proportioning is pressed chemical formula (Yb xSc yY 1-x-y) 2O 3, x in the formula=0.01 ~ 0.15, y=0.10 ~ 0.90;
B. will stir by the good body material of above-mentioned formulated and dopant material mixed,, compound was dissolved in the dehydrated alcohol, with ball mill mix grinding 5 hours.Ball milling is 1:2 with the mass ratio of powder during ball milling, and the ratio of dehydrated alcohol and powder is that every 1g powder adds dehydrated alcohol 5mL, and rotational speed of ball-mill is 50 rev/mins;
C. dry under 90 ℃ of temperature through the compound behind the ball milling, subsequently 1200 ℃ of following pre-burnings 8 ~ 10 hours;
D. the compound after the pre-burning carries out granulation, and depresses to the sheet sample in the 200MPa isostatic cool pressing;
E. said sample is placed molybdenum filament hydrogen furnace or vacuum oven to carry out sintering, sintering range is 1600～1700 ℃, and soaking time is 15～20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Description of drawings
Fig. 1 is same concentrations Yb 3+The Y that mixes 2O 3, Sc 2O 3And (Sc xY 1-x) 2O 3The emmission spectrum of crystalline ceramics.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
Process and the step of present embodiment are described below
1. adopt high-purity Yb 2O 3(99.99%), Y 2O 3(99.99%) and Sc 2O 3(99.99%) nano powder is raw material, and with Y 2O 3And Sc 2O 3Be body material, with Yb 2O 3Be dopant material.Three's mole proportioning is pressed chemical formula (Yb xSc yY 1-x-y) 2O 3, x in the formula=0.01, y=0.099.The molar content of each composition is: Yb 2O 30.010 mol, Sc 2O 30.099 mol, Y 2O 30.891 mol;
2. will stir mixedly by the good body material of above-mentioned formulated and dopant material, compound was dissolved in the dehydrated alcohol, with ball mill mix grinding 5 hours.Ball milling is 1:2 with the mass ratio of powder during ball milling, and the ratio of dehydrated alcohol and powder is that every 1g powder adds dehydrated alcohol 5mL, and rotational speed of ball-mill is 50 rev/mins;
3. dry under 90 ℃ of temperature through the compound behind the ball milling, subsequently 1200 ℃ of following pre-burnings 8 ~ 10 hours;
4. the compound after the pre-burning carries out granulation, and depresses to the sheet sample in the 200MPa isostatic cool pressing;
5. said sample is placed the molybdenum filament hydrogen furnace to carry out sintering, sintering temperature is 1650 ℃, and soaking time is 10 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 2
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.03, y=0.194.The molar content of each composition is: Yb 2O 30.030 mol, Sc 2O 30.194 mol, Y 2O 30.776 mol.The sample sintering temperature is 1700 ℃, and soaking time is 15 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 3
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.03, y=0.291.The molar content of each composition is: Yb 2O 30.030 mol, Sc 2O 30.291 mol, Y 2O 30.679 mol.The sample sintering temperature is 1700 ℃, and soaking time is 15 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 4
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.03, y=0.388.The molar content of each composition is: Yb 2O 30.030 mol, Sc 2O 30.388 mol, Y 2O 30.582 mol.The sample sintering temperature is 1700 ℃, and soaking time is 15 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 5
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.01, y=0.495.The molar content of each composition is: Yb 2O 30.010 mol, Sc 2O 30.495 mol, Y 2O 30.495 mol.The sample sintering temperature is 1700 ℃, and soaking time is 20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 6
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.03, y=0.485.The molar content of each composition is: Yb 2O 30.030 mol, Sc 2O 30.485 mol, Y 2O 30.485 mol.The sample sintering temperature is 1700 ℃, and soaking time is 20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 7
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.05, y=0.475.The molar content of each composition is: Yb 2O 30.050 mol, Sc 2O 30.475 mol, Y 2O 30.475 mol.The sample sintering temperature is 1700 ℃, and soaking time is 20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 8
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.10, y=0.45.The molar content of each composition is: Yb 2O 30.100 mol, Sc 2O 30.450 mol, Y 2O 30.450 mol.Sample places the vacuum oven sintering, and sintering temperature is 1700 ℃, and soaking time is 20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 9
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.15, y=0.425.The molar content of each composition is: Yb 2O 30.150 mol, Sc 2O 30.425 mol, Y 2O 30.425 mol.Sample places the vacuum oven sintering, and sintering temperature is 1700 ℃, and soaking time is 20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 10
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.05, y=0.57.The molar content of each composition is: Yb 2O 30.050 mol, Sc 2O 30.570 mol, Y 2O 30.380 mol.The sample sintering temperature is 1700 ℃, and soaking time is 20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 11
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.05, y=0.665.The molar content of each composition is: Yb 2O 30.050 mol, Sc 2O 30.665 mol, Y 2O 30.285 mol.The sample sintering temperature is 1650 ℃, and soaking time is 15 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 12
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.05, y=0.760.The molar content of each composition is: Yb 2O 30.050 mol, Sc 2O 30.760 mol, Y 2O 30.190 mol.The sample sintering temperature is 1650 ℃, and soaking time is 15 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 13
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.01, y=0.891.The molar content of each composition is: Yb 2O 30.010 mol, Sc 2O 30.891 mol, Y 2O 30.099 mol.The sample sintering temperature is 1650 ℃, and soaking time is 15 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 14
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.03, y=0.873.The molar content of each composition is: Yb 2O 30.030 mol, Sc 2O 30.873 mol, Y 2O 30.097 mol.The sample sintering temperature is 1650 ℃, and soaking time is 15 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 15
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.05, y=0.855.The molar content of each composition is: Yb 2O 30.050 mol, Sc 2O 30.855 mol, Y 2O 30.095 mol.The sample sintering temperature is 1650 ℃, and soaking time is 15 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 16
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.10, y=0.810.The molar content of each composition is: Yb 2O 30.100 mol, Sc 2O 30.810 mol, Y 2O 30.090 mol.The sample sintering temperature is 1600 ℃, and soaking time is 20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Embodiment 17
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is chemical molecular formula (Yb xSc yY 1-x-y) 2O 3In x=0.15, y=0.765.The molar content of each composition is: Yb 2O 30.150 mol, Sc 2O 30.765 mol, Y 2O 30.085 mol.The sample sintering temperature is 1600 ℃, and soaking time is 20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
Crystalline ceramics by the preparation of method described in the above embodiment has good transparency.The emmission spectrum of all ceramics samples is measured via the French J-Y Fluorophog-3 of company fluorescence spectrophotometer, adopts LD pumping source 940 nm wave bands to excite, and it the results are shown in Fig. 1.Yb:(Sc among the present invention as seen from the figure xY 1-x) 2O 3Crystalline ceramics is with respect to Yb:Y 2O 3And Yb:Sc 2O 3, the obvious broadening of its emission peak, the halfwidth (FWHM) at highest peak 1036 nm places increases to 23 nm by 16 ~ 18 original nm, and the Yb of the described method preparation of above embodiment is adopted in this explanation 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic meets in the femtosecond pulse technology fully for the wide requirement of broad emission band, can be as excellent femtosecond pulse material.

Claims (1)

1. Yb who can be used for the femtosecond pulse field 3+(Sc mixes xY 1-x) 2O 3The preparation method of transparent laser ceramic is characterized in that having following technological process and step:
Adopt high-purity 99.99% Yb 2O 3, 99.99% Y 2O 3With 99.99% Sc 2O 3Nano powder is raw material, with Y 2O 3And Sc 2O 3Be body material, Yb 2O 3Be dopant material, three's mole proportioning is pressed chemical formula (Yb aSc bY 1-a-b) 2O 3, a in the formula=0.01 ~ 0.15, b=0.10 ~ 0.90;
To stir mixed by above-mentioned formulated good body material and dopant material, compound is dissolved in the dehydrated alcohol, with ball mill mix grinding 5 hours, ball milling is 1:2 with the mass ratio of powder during ball milling, the ratio of dehydrated alcohol and powder is that every 1g powder adds dehydrated alcohol 5mL, and rotational speed of ball-mill is 50 rev/mins;
Dry under 90 ℃ of temperature through the compound behind the ball milling, subsequently 1200 ℃ of following pre-burnings 8 ~ 10 hours;
Compound after the pre-burning carries out granulation, and depresses to the sheet sample in the 200MPa isostatic cool pressing;
Place molybdenum filament hydrogen furnace or vacuum oven to carry out sintering said sample, sintering range is 1600～1700 ℃, and soaking time is 15～20 hours, the final transparent Yb of densification that obtains 3+(Sc mixes xY 1-x) 2O 3Transparent laser ceramic.
CN 201110154903 2011-06-10 2011-06-10 Yb<3+>-doped (ScxY1-x)2O3 laser transparent ceramic applicable to femtosecond pulse laser and preparation method thereof Expired - Fee Related CN102320834B (en)

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CN104478433A (en) * 2014-12-08 2015-04-01 上海大学 Nd<3+> doped (Y1-xScx)2O3 laser transparent ceramic and preparation method thereof
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