CN101333110B - Method for preparing Nd<3+> -doped Lu2O3transparent laser ceramic - Google Patents

Method for preparing Nd<3+> -doped Lu2O3transparent laser ceramic Download PDF

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CN101333110B
CN101333110B CN2008100406236A CN200810040623A CN101333110B CN 101333110 B CN101333110 B CN 101333110B CN 2008100406236 A CN2008100406236 A CN 2008100406236A CN 200810040623 A CN200810040623 A CN 200810040623A CN 101333110 B CN101333110 B CN 101333110B
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ceramic
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nitrate
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CN101333110A (en
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施鹰
周鼎
谢建军
云平
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a method for preparing an Nd<3+>-doped Lu2O3 transparent laser ceramic, belonging to the technical field of rare earth metal element optical transparent ceramic preparation technology. The invention adopts a compound precipitating agent solution containing ammonia and ammonium bicarbonate with a weight ratio of 1:1-3. Through a titration method, the compound precipitating agent solution is dripped into a mixed solution of lutetium nitrate and neodymium nitrate. A molar mass ratio of the Lu<3+> and Nd<3+> in the mixed solution is on a basis of a chemical molecular formula (Lu[1-x]Ndx )2O3, x is the molar ratio and the value thereof is 0.05<x<0.1, namely Lu<3+>:Nd<3+>= (1-x): x. In the method of the invention, an Nd<3+>: Lu2O3 precipitation is firstly obtained, deposited, a ceramic powder is obtained after washing, drying and calcination at 1000 DEG C; then the powder is molded by a steel mold through a double compaction, and is sintered under non-pressure in a flowing hydrogen atmosphere with a sintering temperature of 1850-1880 DEG C and a sintering time of 6-10 hours; finally the highly transparent Nd<3+>:Lu2O3 laser ceramic is obtained.

Description

Nd 3+The Lu of ion doping 2O 3The preparation method of transparent laser ceramic
Technical field
The present invention relates to a kind of Nd 3+The Lu of ion doping 2O 3The preparation method of transparent laser ceramic belongs to thulium optical clear pottery fabricating technology field.
Background technology
Along with the fast development of photoelectron and information detection technology, transparent ceramic material more and more shows its unique advantage.Crystalline ceramics has good mechanical, thermal property, and outstanding stability and corrosion resistance nature have the transparent optical property of glass height again.And large-sized monocrystalline material growth production cycle is long, the cost height, special in the novel optical function material with complicated dopant states, traditional crystal technique is difficult to realize the high density and the uniform distribution of dopant ion, and then can't realize the optical property optimization of material.Ceramic nano-powder body technology of preparing and various advanced persons' densifying method provides effective way for preparation optical grade ceramic laser material.Crystalline ceramics preparation technology is simple, is being lower than Lu 2O 3The high densification crystalline ceramics be can obtain under the temperature that the temperature of material melting point (～2490 ℃) is 700 ℃, mass, low cost production are easy to realize.Particularly can require to realize the even doping of high concentration ion according to device application, this raising to the design of material and optical property is most important more conveniently.Japan scholar report, under specific component, the performance of crystalline ceramics has has met or exceeded monocrystal material, is expected in some specific occasions progressively substitute monocrystalline.
Lutecium oxide (Lu 2O 3) have extremely good physical and chemical stability, no moisture absorption and a deliquescence phenomenon.Lu 2O 3Band gap very wide (6.5ev) can hold many activator ions such as Nd as the optical material matrix between valence band and conduction band 3+, Yb 3+, Tm 3+, Eu 3+Deng emission level.Lu 2O 3Its thermal conductivity of body material (12.5W/mk) is slightly higher than current widely used YAG base laserable material (11W/mk), and thermal conductivity is constant substantially after mixing light emitting ionic has high heat conductance (be better than YAG base laserable material), low thermal coefficient of expansion, a low effective phonon energy, by mixing Nd 3+Ion or Yb 3+Ion can prepare the Solid State Laser working medium, is used for superpower ceramic laser device.
In sum, Lu 2O 3Be a kind of extremely promising laserable material matrix.Yet Lu 2O 3Fusing point is up to 2490 ℃, and the employing Czochralski grown contains the not only difficult realization of technology of monocrystal material of various doping components, and cost is quite high.Lu 2O 3Have cubic crystal structure, optical isotropy can prepare the laser ceramics of high compaction by nanocrystalline technology and reducing atmosphere pressureless sintering technology.Therefore developing the lutecia based transparent ceramics material is that this class material obtains key in application.And the key that obtains transparent ceramic material is to prepare the high nano-powder of sintering activity earlier, requires the powder granule size little, even particle size distribution, the spherical in shape and good dispersity of particle.The wet chemistry method coprecipitation technology is one of the feasible method of realizing this goal.
Up to the present, about Nd 3+: Lu 2O 3The bibliographical information of laserable material seldom.The current seminar that carries out lutecium oxide ceramic powder preparation research in the world mainly contains Polish E.Zych and Japanese J.Lu, K.Ueda study group.2002, people such as J.Lu adopted the urea precipitation from homogeneous solution (PFHS) to prepare powder, and vacuum sintering has prepared 0.15at.%Nd then 3+: Lu 2O 3Ceramic laser material, but relevant Nd 3+: Lu 2O 3Powder preparing, sintering method and Lu 2O 3Every performance of transparent material does not have the details report.2005, K.Takaichi etc. reported the 3at.%Yb:Lu that adopts vacuum sintering and the preparation of nanocrystalline technology 2O 3Laser ceramics, its powder preparation method are not reported details equally.Can mainly contain Polish E.Zych for the preparation of other rare earth ion doped lutecium oxide powder of using for reference.2002, E.Zych etc. utilized urea to make fuel with the synthetic RE of solution combustion method 3+Adulterated Lu 2O 3Luminescent powder obtains translucent ceramics sample through 1700 ℃ of vacuum sinterings 5 hours, and this is that at high temperature annealing back grain growth is obvious because the burning synthetic powder is reunited seriously, thereby the sintering activity that has reduced powder is low.2004, this study group reported melting salt method (molten salts route) preparation Eu 3+: Lu 2O 3The method of luminescence nanocrystalline, IR spectrum shows the Lu of cube phase 2O 3A small amount of OH is arranged in the matrix -Ion is remaining, and grain-size is at 18～30nm.Studies show that (NO with Lu 3) 3Preparation is than using LuCl 3The nano powder luminescent properties height of preparation; The pressureless sintering technology prepares crystalline ceramics requirement powder and has good dispersiveness and high sintering activity.The same year, E.Zych etc. have studied the burning urea method and the Pechini legal system is equipped with the lutecium oxide powder, the morphology microstructure that two kinds of methods obtain is similar, and to calculate the lutecium oxide powder granule size of Pechini method preparation as can be known little but rein in formula according to XRD scanning halfwidth by seat, and spectrum property is good.In addition, the powder with burning urea method preparation is higher than at 3% o'clock at the Eu doping content, the concentration quenching phenomenon takes place and is preparing the lutecium oxide powder at Eu with the Pechini method 3+Ion doping content reaches at 10% o'clock concentration quenching does not all take place.Subsequently, this study group is again to Eu 3+: Lu 2O 3The composite mixed Mg of luminescent powder, Ca, Sr, Ba, La are through 1750 ℃, and what vacuum sintering in 5 hours was done studies show that: doped with Mg 2+The block transparency of ionic powder sintering is relatively poor, doping Ca 2+Ion can promote partially transparent, doping Sr 2+, Ba 2+, La 3+Ion can promote the block transparency.
At Lu 2O 3Block laser activity aspect: in October, 2002, J.Lu etc. have reported that employing vacuum sintering and nanocrystalline technology of preparing prepare the adulterated Nd:Lu of 0.15at.% first 2O 3Crystalline ceramics, and realized laser output.Sample adopts the urea homogeneous precipitation method to prepare nano-powder, and gypsum mould grouting is shaped the back in 1700 ℃ of vacuum sinterings acquisition in 5 hours Nd:Lu then 2O 3Crystalline ceramics.The ceramics sample of laser test is of a size of 6mm * 6mm * 1mm, not plated film.Spectral investigation shows Nd:Lu 2O 3Polycrystalline ceramics has two obvious absorption peaks at wavelength 807nm and 822nm place, corresponding to 4F 2/3→ 4I 11/2Energy level transition.Owing to lack and the Wavelength matched laser apparatus of 822nm, use wavelength to be the 807nm semiconductor laser pumping in the test.When pump power reached 1W, the energy of absorption of sample 185mW had also obtained the laser output of 10mW, slope efficiency 13.3%.2005, K.Takaichi etc. reported the 3at.%Yb:Lu that adopts vacuum sintering and the preparation of nanocrystalline technology 2O 3Ceramic laser.In the experimentation, Yb 3+: Lu 2O 3Ceramic plate thickness is 1mm, and the LD pump power of modified optical fiber is 5W, excites following maximum absorption to be 2.6W at 1035nm and the lasting wavelength of 1079nm, and output rating is respectively 0.7W and 0.95W, and slope efficiency reaches 36% and 53%. 2F 5/2Fluorescence lifetime is about 1.02 ± 0.01ms, and its performance can compare favourably with monocrystalline.
From above situation, have not yet to see the composite precipitation method and prepare Nd:Lu in conjunction with pressureless sintering 2O 3The report of transparent laser ceramic.
Summary of the invention
The object of the present invention is to provide a kind of composite precipitation legal system to be equipped with Nd 3+The Lu of ion doping 2O 3Nano-powder and under nitrogen atmosphere pressureless sintering prepare Nd 3+: Lu 2O 3The method of transparent laser ceramic.
A kind of Nd of the present invention 3+The Lu of ion doping 2O 3Transparent laser ceramic is characterized in that having following chemical molecular formula:
(Lu 1-xNd x) 2O 3
X represents the mole component of dopant ion, and 0≤x≤0.20.
Described chemical molecular formula (Lu 1-xNd x) 2O 3In, the optimum value of the mole component of dopant ion is: 0.005≤x≤0.1.
A kind of Nd of the present invention 3+The Lu of ion doping 2O 3The preparation method of transparent laser ceramic is characterized in that having following preparation process and step:
A. at first highly purified lutecium nitrate and neodymium nitrate are dissolved in respectively in the deionized water, constitute the aqueous solution of lutecium nitrate and neodymium nitrate, prepare the mixing solutions of lutecium nitrate and neodymium nitrate subsequently according to x mole component value in the above-mentioned molecular formula, and make Lu in the solution 3+With Nd 3+Ionic molar mass ratio is x: (1-x), and 0.005≤x≤0.1 wherein;
B. prepare the composite precipitation agent solution: the ratio of ammoniacal liquor and bicarbonate of ammonia 1: 1 by weight ratio～3 is prepared alkaline composite precipitation agent solution;
C. above-mentioned composite precipitation agent solution slowly is titrated in the beaker that fills lutecium nitrate and neodymium nitrate mixing solutions, vigorous stirring, rate of titration are 2～5ml/ branch, and the pH value of titration end point is controlled between 8～9, titration finishes the back and continues to stir for some time, forms the precipitation presoma;
D. will precipitate presoma in room temperature ageing 24～48 hours, use circulation ability of swimming vacuum pump suction filtration then, use deionized water wash subsequently 2～3 times; The filter cake of gained behind the suction filtration is scattered in the dehydrated alcohol, stirs,, so repeat 2～3 times to clean foreign ion with suction filtration again behind the ultra-sonic dispersion;
E. with the precipitation presoma of above-mentioned washes clean in 90 ℃ dry 24 hours down, will precipitate presoma then and calcine 2 hours in 1000 ℃; Furnace cooling obtains Nd 3+: Lu 2O 3Nano-ceramic powder;
F. above-mentioned ceramic powder is placed in the punching block biscuit earlier with the two-way φ of the being suppressed into 20mm of the pressure of 20～50MPa; Under 100～300MPa pressure, carry out the isostatic cool pressing compacting again, obtain the biscuit of high-compactness;
G. place the reducing atmosphere of flowing hydrogen to carry out pressureless sintering above-mentioned high-compactness biscuit, rise to 1850～1880 ℃, and under this sintering temperature, be incubated 6～10 hours with 2～5 ℃/min temperature rise rate; 1350 ℃ of annealing 2 hours in air atmosphere more finally obtains the Nd of highly transparent subsequently 3+Adulterated Lu 2O 3Transparent laser ceramic.
Adopt compound precipitants in the inventive method, wherein an amount of having of carbanion is beneficial to the reduction particle aggregation, and obtains powder with higher sintering activity.In addition, adopt normal pressure nitrogen atmosphere sintering, also help obtaining the laser ceramics body of highly transparent.
Description of drawings
Fig. 1 is 3mol%Nd in the embodiment of the invention 3+Ion doping Lu 2O 3X-ray diffraction (XRD) collection of illustrative plates after presoma is calcined under differing temps.
Fig. 2 is Nd 3+Doping Lu 2O 3Specific surface area (the S of nano-powder BET) and grain-size (d BET) and calcining temperature between graph of relation.
Fig. 3 among the present invention at 1000 ℃ of calcinings Nd after 2 hours 3+: Lu 2O 3The scanning electron microscope of powder (SEM) shape appearance figure.
Fig. 4 is for precipitating transmission electron microscope (TEM) shape appearance figure of presoma in 1000 ℃ of calcinings powder after 2 hours among the present invention.
The Nd of Fig. 5 after for the surface finish among the present invention 3+: Lu 2O 3Transparent optical ceramics sample photo in kind.This thickness of sample is 1.4mm, has the good optical transparency.
The Nd of Fig. 6 after for the surface finish among the present invention 3+: Lu 2O 3The crystalline ceramics sample is in the transmittance curve figure of visible light wave range.
Fig. 7 is Nd of the present invention 3+: Lu 2O 3The optical microscope photograph of crystalline ceramics glazed surface and fresh fracture scanning (SEM) shape appearance figure.
Fig. 8 is the high-resolution-ration transmission electric-lens photo of crystalline ceramics sample of the present invention.
Fig. 9 is the 3mol%Nd:Lu of embodiment of the invention gained 2O 3Crystalline ceramics is emmission spectrum figure under the 808nm condition at excitation wavelength.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment one: preparation 3.0mol.%Nd:Lu 2O 3Laser transparent ceramic
Get the Lu (NO of 200ml 0.964mol/L 3) 3Nd (NO with 4.8ml 1.199mol/L 3) 3The beaker that places 3000ml, regulating starting point concentration is that 0.1mol/L is standby.Get 33.3ml analytical pure ammoniacal liquor, the ammonium bicarbonate soln uniform mixing of 1000ml 2mol/L standby in the Plastic Bottle of 2.5L (about 1mol/L).Adopt and just dripping method, the alkaline solution that configures is titrated to Lu with 3ml/min speed with plough type funnel 3+And Nd 3+In the ionic mixing solutions, the while vigorous stirring, the pH value of titration end point is controlled to be about 9, titration finishes to continue to stir 120min, to precipitate presoma after room temperature leaves standstill 48 hours with circulation ability of swimming vacuum pump suction filtration, deionized water wash 2 times, get filter cake and be dissolved in the dehydrated alcohol, suction filtration again behind the ultra-sonic dispersion, repeat 2-3 all over to clean foreign ion, the filter cake that finally obtains is placed the dry 24h of 90 ℃ in baking oven.Difference is calcined 2h for 1000 ℃ in retort furnace afterwards, and furnace cooling promptly gets required nano-powder.Dry-pressing is adopted in the powder moulding, waits static pressure then.The two-way biscuit that is pressed into Φ 20mm of punching block is adopted in dry-pressing, and forming pressure 30MPa waits static pressure to adopt oil bath, forming pressure 200MPa.At last, the biscuit after the moulding places hydrogen furnace by the reducing atmosphere non-pressure sintering technology, is incubated 6h under 1850 ℃ temperature, can obtain the 3mol.%Nd of highly transparent 3+Doping Lu 2O 3Base transparent optical pottery.
Embodiment two: 3mol%Nd:Lu 2O 3Crystalline ceramics (the anti-method of dripping)
It is standby in the beaker of 1000ml to get the mixed precipitant 250ml for preparing among the embodiment one.Lu (NO with 50ml 0.964mol/L 3) 3Nd (NO with 1.2ml 1.199mol/L 3) 3Solution mix and place 500ml plough type funnel, to above-mentioned alkaline solution, the titer in the control plough type funnel makes that the final PH of solution is controlled at about 9 in the beaker, must precipitate presoma with the speed titration of 3ml/min.The ageing of presoma, washing, processes such as suction filtration, moulding and sintering method are with embodiment one.
Embodiment three: preparation 0.5mol%Nd:Lu 2O 3Laser transparent ceramic
Get the Lu (NO of 200ml 0.964mol/L 3) 3Nd (NO with 0.804ml 1.199mol/L 3) 3Solution places the beaker of 3000ml, and regulating starting point concentration is that 0.15mol/L is standby.Use compound precipitants 3ml/min speed titration according to above method configuration.The titration final pH of solution that finishes is controlled at about 8.5, the ageing of presoma, washing, suction filtration, calcining and moulding process are with embodiment one, biscuit after the moulding places hydrogen furnace by reducing atmosphere pressureless sintering method, be incubated 10h under 1880 ℃ temperature, sample can obtain the good 0.5mol.%Nd of optical transparence behind the annealing 2h under 1350 ℃ of conditions in air atmosphere subsequently 3+: Lu 2O 3Transparent laser ceramic.
Embodiment four: preparation 10.0mol%Nd:Lu 2O 3Laser transparent ceramic
Get the Lu (NO of 200ml 0.964mol/L 3) 3Nd (NO with 16.080ml 1.199mol/L 3) 3The beaker that places 3000ml, regulating starting point concentration is that 1mol/L is standby.Use compound precipitants 3ml/min. speed titration according to above method configuration.Titration preparation such as after scouring, oven dry, moulding and the sintering laser ceramicses that finish are identical with embodiment one.
Gained Nd in the embodiment of the invention 3+: Lu 2O 3The instrument detecting of sample
(1) 1.5mol%Nd 3+: Lu 2O 3The X fluorescence spectrum composition analysis of powder, its detected result sees the following form 1.
Table 1Nd 3+: Lu 2O 3The X fluorescence spectrum composition analysis of powder
Content mol%
Nd 2O 3 1.732
Lu 2O 3 98.268
(2) Nd 3+: Lu 2O 3Biscuit is in dry-pressing and wait sample density detection in the static pressure process, and its detected result sees the following form 2.
Table 2Nd 3+: Lu 2O 3The density of biscuit behind dry-pressing and static pressure such as grade
After dry-pressing formed Behind the static pressure such as 200MPa
Biscuit density (g/cm 3) 3.53 4.45
Biscuit relative density (%) 37.8 47.6
3mol%Nd in the embodiment of the invention 3+Ion doping Lu 2O 3X-ray diffraction (XRD) collection of illustrative plates under the presoma differing temps after the calcining is seen Fig. 1.
Nd in the embodiment of the invention 3+Doping Lu 2O 3The specific surface area (S of nano-powder BET) and grain-size (d BET) and calcining temperature between relation see Fig. 2.
In the embodiment of the invention, 1000 ℃ the calcining 2 hours after Nd 3+: Lu 2O 3The pattern of the scanning electron microscope of powder (SEM) is seen Fig. 3; Visible in the drawings its grain-size is 40～60nm, and favorable dispersity.
In the embodiment of the invention, the precipitation presoma is seen Fig. 4 in transmission electron microscope (TEM) pattern of 1000 ℃ of calcinings powder after 2 hours; In the drawings as seen, average grain size is 40nm, and does not have serious agglomeration.
Nd after the surface finish in the embodiment of the invention 3+: Lu 2O 3Transparent optical ceramics sample photo in kind is seen Fig. 5.This thickness of sample is 1.4mm, and it has the good optical transparency.
Nd after the surface finish in the embodiment of the invention 3+: Lu 2O 3The crystalline ceramics sample is seen Fig. 6 in the transmitance of visible light wave range.Show among the figure that its transmitance reaches more than 70%.
The Nd that the embodiment of the invention obtains 3+: Lu 2O 3The optical microscope photograph of crystalline ceramics glazed surface and fresh fracture scanning (SEM) pattern are seen Fig. 7.
The high resolving power transmission electron microscope photo of embodiment of the invention gained crystalline ceramics sample is seen Fig. 8; Among the figure as seen, adjacent Lu 2O 3The intergranule contact is tight, and two-phases such as no crystal boundary are separated out.
Embodiment of the invention gained 3mol%Nd:Lu 2O 3Crystalline ceramics is that emmission spectrum under the 808nm condition is seen Fig. 9 at excitation wavelength.

Claims (1)

1. Nd 3+The Lu of ion doping 2O 3The preparation method of transparent laser ceramic, the molecular formula of this transparent laser ceramic is: (Lu 1-xNd x) 2O 3, X represents the mole component of dopant ion, and 0≤x≤0.20, it is characterized in that having following preparation process and step:
A. at first highly purified lutecium nitrate and neodymium nitrate are dissolved in respectively in the deionized water, constitute the aqueous solution of lutecium nitrate and neodymium nitrate, prepare the mixing solutions of lutecium nitrate and neodymium nitrate subsequently according to x mole component value in the above-mentioned molecular formula, and make Nd in the solution 3+With Lu 3+Ionic molar mass ratio is x: (1-x);
B. prepare the composite precipitation agent solution: the ratio of ammoniacal liquor and bicarbonate of ammonia 1: 1 by weight ratio～3 is prepared alkaline composite precipitation agent solution;
C. above-mentioned composite precipitation agent solution slowly is titrated in the beaker that fills lutecium nitrate and neodymium nitrate mixing solutions, vigorous stirring, rate of titration are 2～5 ml/min, and the pH value of titration end point is controlled between 8～9, titration finishes the back and continues to stir for some time, forms the precipitation presoma;
D. will precipitate presoma in room temperature ageing 24～48 hours, use circulation ability of swimming vacuum pump suction filtration then, use deionized water wash subsequently 2～3 times; The filter cake of gained behind the suction filtration is scattered in the dehydrated alcohol, stirs,, so repeat 2～3 times to clean foreign ion with suction filtration again behind the ultra-sonic dispersion;
E. with the precipitation presoma of above-mentioned washes clean in 90 ℃ dry 24 hours down, will precipitate presoma then and calcine 2 hours in 1000 ℃; Furnace cooling obtains Nd 3+: Lu 2O 3Nano-ceramic powder;
F. above-mentioned ceramic powder is placed in the punching block biscuit earlier with the two-way φ of the being suppressed into 20mm of the pressure of 20～50MPa; Under 100～300MPa pressure, carry out the isostatic cool pressing compacting again, obtain the biscuit of high-compactness;
G. place the reducing atmosphere of flowing hydrogen to carry out pressureless sintering above-mentioned high-compactness biscuit, rise to 1850～1880 ℃, and under this sintering temperature, be incubated 6～10 hours with 2～5 ℃/min temperature rise rate; 1350 ℃ of annealing 2 hours in air atmosphere more finally obtains the Nd of highly transparent subsequently 3+Adulterated Lu 2O 3Transparent laser ceramic.
CN2008100406236A 2008-07-16 2008-07-16 Method for preparing Nd<3+> -doped Lu2O3transparent laser ceramic Expired - Fee Related CN101333110B (en)

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CN101787279A (en) * 2010-03-04 2010-07-28 上海大学 Solvent thermal synthesis method of Lu2O3 nanorod luminescent powder
CN102557598B (en) * 2011-03-21 2014-10-01 上海大学 Pressureless sintering preparation method of Ce:Lu2SiO5 polycrystal flicker optical ceramics
CN102674837A (en) * 2012-05-22 2012-09-19 长春理工大学 Er<3+>:Lu2O3 transparent ceramic
CN102807368B (en) * 2012-09-03 2014-06-11 上海应用技术学院 Preparation method of Nd<3+>:Lu2O3 translucent nano ceramic
CN106145959B (en) * 2016-07-10 2018-08-17 九江学院 A kind of preparation method of luteium oxide crystalline ceramics
CN108977882B (en) * 2018-08-31 2021-02-12 山东大学 Sesquioxide single crystal optical fiber and preparation method and application thereof
US20220200231A1 (en) * 2019-01-25 2022-06-23 The Regents Of The University Of California Rare-earth-doped alumina-oxide laser gain media
CN116354721A (en) * 2023-03-24 2023-06-30 沈阳大学 Activated ion concentration continuous gradient distribution lutetium oxide laser transparent ceramic material and preparation method thereof

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