CN102882118A - Transparent colloid laser medium and preparation method thereof - Google Patents
Transparent colloid laser medium and preparation method thereof Download PDFInfo
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- CN102882118A CN102882118A CN201210370910XA CN201210370910A CN102882118A CN 102882118 A CN102882118 A CN 102882118A CN 201210370910X A CN201210370910X A CN 201210370910XA CN 201210370910 A CN201210370910 A CN 201210370910A CN 102882118 A CN102882118 A CN 102882118A
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Abstract
The invention belongs to the field of laser materials, and particularly relates to a transparent colloid laser medium and a preparation method thereof. By means of the preparation method, rare-earth salts and villiaumite serve as the raw materials, and rare-earth activated ion doped rear-earth nanometer crystals controllable in grain size are prepared in a wet chemistry method; organic ligands are used for performing sensitization on the surface of the rear-earth nanometer crystals; and the sensitized rear-earth nanometer crystals are dispersed in heavy water or organic medium, so that the novel transparent colloid laser medium is prepared. Compared with the traditional solid laser media, the liquid transparent colloid laser medium is remarkably improved in thermal conductivity, and remits the problem of temperature gradient, and a liquid laser constructed by the laser medium cannot be damaged easily and has good optical performance.
Description
Technical field
The present invention relates to a kind of laser medium technology of preparing, relate to particularly a kind of transparent colloid laser medium and preparation method thereof, belong to the laser material field.
Background technology
High repetition High-power Laser Technologies is one of significant development direction of laser technology, and important role on the fields such as human future new forms of energy, national economic development, scientific research especially has very high strategic importance at the construction tactical laser weapons.For example the U.S. building 192 the bundle, 1.8 megajoule pulse energies national ignition installation (NIF), 60 bundles that China is developing, the huge device of Shenguang-Ⅲ main frame of 100KJ etc., except in some fraction field search gas laser, what major part all adopted is Solid State Laser, uses solid laser medium.
At present because the solid strong laser system adopts solid laser medium to run into inevitably some difficulties and technical bottleneck.The one, solid laser material is easy injury point in high-power operation, and in case generate impaired loci, can enlarge rapidly in high power operation, finally cause the destruction of self, this has become the very severe natural bottleneck that laser operation power continues lifting; The 2nd, the thermal effect of solid state laser laser medium under the high power conditions operation, owing to there is not preferably cooling scheme, can't fundamentally reduce used heat, thereby affect the Laser output of high repetition, high light beam quality, also just limited its repeat usage, the scope of application, service cycle and useful life; Make simultaneously operating cost high, do not reach the requirement of large-scale commercial applications production.
Summary of the invention
The object of the invention is to propose a kind of technical bottleneck that can overcome present solid laser medium easy damaged and poor thermal conductivity, a kind of transparent colloid new pattern laser medium and preparation method thereof is provided.The method is to add rare-earth salts successively in the mixed solution that contains solvent and surfactant, add subsequently villiaumite and get composite solution, in water heating kettle, react rare earth doped nanocrystallinely, with organic ligand with the rare earth doped nanocrystalline sensitization of carrying out, with rare earth doped nanocrystalline being scattered in the organic media after the sensitization, namely make transparent colloid new pattern laser medium at last.
For achieving the above object, the present invention adopts the technical scheme of following technical measures formation to realize.
The preparation method of a kind of transparent colloid laser medium that the present invention proposes is characterized in that comprising successively following processing step:
(1) the preparation rare earth activation ion is rare earth doped nanocrystalline
In the mixed solution that contains solvent and surfactant, add rare-earth salts, stirred 10~30 minutes; Add subsequently villiaumite and get composite solution, regulate its pH value 6~9, stirred 10~60 minutes; Again composite solution is transferred in the water heating kettle, 160~230 ℃ of lower reactions 6~36 hours; Add ethanol or cyclohexane collecting precipitation, centrifugation, drying is 24 hours in 60 ℃ baking oven, and it is rare earth doped nanocrystalline namely to make rare earth activation ion;
(2) remove rare earth doped nanocrystal surface activating agent
The rare earth doped nanocrystalline concentration with 0.2g/L~2.0g/L of the rare earth activation ion that at room temperature step (1) is made is dispersed in and gets mixed solution in methyl alcohol and the chloroform, described mixed solution slowly is added drop-wise in acidity or the alkaline chloroformic solution, sonic oscillation 4~8 hours, under vacuum condition, remove unnecessary methyl alcohol and chloroform, remove the activating agent of rare earth doped nanocrystal surface;
(3) utilize the organic ligand sensitization rare earth doped nanocrystalline
Rare earth doped nanocrystallinely join sensitization in the ethanolic solution that contains organic part with what step (2) was removed surfactant, under 60~140 ℃ of temperature conditions, refluxed 2~8 hours, revolve to steam after reaction is finished and remove unnecessary alcohol;
(4) acquisition of transparent colloid working-laser material
With ethanol and deionized water with the reacted rare earth doped nanocrystalline cyclic washing of step (3) three times, drying is 48 hours in 60 ℃ baking oven, again dried rare earth doped manocrystalline powders is dispersed in the organic media in heavy water or deuterium generation, namely obtains the transparent colloid working-laser material.
In the such scheme, described rare-earth salts is rare earth nitrades or rare earth-iron-boron, and described villiaumite is sodium fluoride or ammonium fluoride or bifluoride hydrogen ammonia; Prepared rare earth activation ion rare earth doped nanocrystalline be the fluoride of lanthanum, cerium, praseodymium, neodymium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium; Or oxide; Or phosphate; Or vanadate, or fluoride is received salt.
In the such scheme, described rare earth activation ion is neodymium or europium or holmium or erbium or thulium or rare earth activation ion pair; Described rare earth activation ion is to being ytterbium/dysprosium or ytterbium/holmium or ytterbium/erbium or ytterbium/thulium; The percentage that described rare earth activation ion consumption accounts for total rare earth (TRE) ionic species amount is 1~25%.
In the such scheme, described organic ligand is benzoic acid or tropolone or hexanitrodiphenyl amine or beta-diketon class, and described beta-diketon class is pentanedione or Phen or bipyridine or trifluoroacetylacetone (TFA).
In the such scheme, described deuterium is that deuterated methanol or deuterated acetone or deuterium are for DMF or deuterated dimethyl sulfoxide for organic media.
In the such scheme, described solvent is deionized water, methyl alcohol or ethanol or ethylene glycol or diethylene glycol or octadecylene; Described surfactant is polymine or polyvinylpyrrolidone or polyacrylic acid or oleic acid or citric acid or ethylenediamine tetra-acetic acid or ten hexamethyl trimethylammonium bromides.
The fluid state laser that the prepared transparent colloid laser medium of the present invention makes up is characterized in that comprising the diode-end-pumped source, first lens, the second lens, plano-concave mirror, the laser medium circulatory system, average mirror; The laser of described diode-end-pumped source output, incide the laser medium circulatory system behind the 4f system collimation that process first lens and the second lens consist of, laserresonator is made of plano-concave mirror and average mirror, and the plano-concave mirror is input mirror, and average mirror is outgoing mirror.
In the such scheme, the described laser medium circulatory system is by the laser medium fixture, adpting flange, and flexible pipe, the transparent colloid liquid reserve tank, circulating pump forms; The described laser medium circulatory system is by the laser medium fixture, adpting flange, and flexible pipe, the transparent colloid liquid reserve tank, circulating pump forms; Described laser medium fixture is connected with flexible pipe by adpting flange, and flexible pipe is connected with the transparent colloid liquid reserve tank, and the transparent colloid liquid reserve tank injects the transparent colloid in the case laser medium fixture and transparent colloid is circulated by circulating pump.
In the such scheme, described laser medium fixture is comprised of the first filming titanium jewel disk, the second plated film titanium jewel sheet, conduit, copper coin sheet and sealing ring; The first filming titanium jewel disk and the second plated film titanium jewel disk separate by sealing ring, and it forms microcavity between the two, and conduit and copper coin sheet are tightly connected.
Rare earth activation ion consumption of the present invention accounts for the percentage of total rare earth (TRE) ionic species amount, and wherein, described total rare earth (TRE) ionic species amount refers to the total amount of rare earth ion contained in the rare earth activation ion that mixes and the rare earth doped nanocrystalline matrix.
The purpose that the present invention carries out sensitization to rare earth doped nanocrystal surface is for strengthening the fluorescence intensity of inorganic nano-crystal, reducing or to eliminate the nanocrystal surface quenching group to its radiationless transition that causes, thereby improves its rare earth doped nanocrystalline fluorescence lifetime.
The present invention have good flowability and high thermal conductivity, thereby its temperature gradient explained is eased according to the transparent colloid laser medium that said method prepares; The fluid state laser that utilizes this transparent colloid laser medium to make up is not prone to damage, and it has higher fluorescence quantum efficiency and good optical property; With the fluid state laser that this transparent colloid laser medium is made, can be widely used in numerous association areas such as the national defence that needs laser, communication.
Description of drawings
Fig. 1 is the structural representation that the prepared transparent colloid laser medium of the present invention is used for the fluid state laser of structure;
Fig. 2 is the structural representation of the laser body medium circulatory system in the fluid state laser described in Fig. 1;
Fig. 3 is fixed laser medium schematic diagram in the circulatory system of laser medium described in Fig. 2.
Among the figure, 1 diode-end-pumped source, 2 first lens, 3 second lens, 4 flat-concave mirrors, the 5 laser medium circulatory systems, 6 average mirrors, 7 laser medium fixtures, 8 adpting flanges, 9 flexible pipes, 10 transparent colloid liquid reserve tanks, 11 circulating pumps, 12 plated films the first titanium jewel disk, 13 conduits, 14 plated films the second titanium jewel disk, 15 copper coin sheets, 16 sealing rings.
Embodiment
Below by specific embodiment the present invention is prepared the transparent colloid laser medium and be described in further detail, but should not be understood as any restriction of the present invention being protected Composition of contents.
Embodiment 1: the preparation (LaF that transparent colloid neodymium doping lanthanum fluoride is nanocrystalline
3: Nd)
9 ml octadecylenes, 10 ml ethanol and 20 ml oleic acid are mixed, add the altogether rare earth nitrades of 1 mmol, wherein (Ln (NO to this solution under stirring
3)
3, Ln:95 mol% La, the 5 mol% Nd aqueous solution stirred 10 minutes; Add again 4ml NH
4F (1.0M) aqueous solution, adding subsequently 3mol/l ammoniacal liquor adjusting pH is 6, stirs 10 minutes to get mixed solution; Described mixed solution is transferred in the 50 ml water heating kettles, and hydrothermal treatment consists is 6 hours under 160 ℃ of temperature conditions; Naturally after the cooling, add the cyclohexane collecting precipitation, and separate with centrifuge; Then use ethanol and deionized water cyclic washing three times, drying is 24 hours in the baking oven of 60 ℃ of temperature; It is nanocrystalline with the neodymium doping lanthanum fluoride of oleic acid to obtain the surface;
With the LaF of 0.06g surface with oleic acid
3: Nd joins the methyl alcohol of 60 ml: chloroform is 1:1, in the mixed solvent of v/v, be slowly to drip described mixed solution in 3 the chloroformic solution to the pH that contains hydrochloric acid, with this composite solution after ultrasonic 4 hours, under vacuum condition, remove unnecessary methyl alcohol and chloroform, and with ethanol and deionized water cyclic washing three times, join subsequently in the ethanolic solution of Phen, under 60 ℃ of temperature conditions, refluxed 2 hours, cooling, revolve to steam and remove unnecessary alcohol, water and ethanol washing three times obtained rare earth doped manocrystalline powders in dry 48 hours under 60 ℃ of temperature conditions, this powder ultrasonic is distributed in the heavy water, it is nanocrystalline to obtain transparent colloid neodymium doping lanthanum fluoride, is prepared transparent colloid laser medium.
Embodiment 2: the preparation (NaGdF of transparent colloid neodymium doping gadolinium tetrafluoride natrium nanocrystalline
4: Nd)
9 ml deionized waters, 10 ml ethanol and 0.4g ethylenediamine tetra-acetic acid are mixed, add the altogether rare earth-iron-boron (Lncl of 1 mmol 0.5mol/L to this solution under stirring
3, Ln:95 mol% Gd, the 5 mol%Nd aqueous solution stirred 30 minutes, added subsequently 4ml NaF (1.0M) aqueous solution again, added NaOH and regulated pH most 9, stirred 60 minutes.Mixed solution is transferred to 50 ml water heating kettles, in 230 ℃ of hydrothermal treatment consists 36 hours.Naturally cool off, add the ethanol collecting precipitation, and separate with centrifuge, wash three times with ethanol and deionized water, drying is 24 hours in 60 ℃ of baking ovens.Can obtain the surface with the neodymium doping gadolinium tetrafluoride natrium nanocrystalline of ethylenediamine tetra-acetic acid.
With the NaGdF of 0.18g surface with ethylenediamine tetra-acetic acid
4: Nd joins the methyl alcohol of 60 ml: chloroform (1:1, v/v) in the mixed solvent, in the chloroformic solution that contains hydrochloric acid (pH=6), slowly drip above-mentioned mixed solution, with ultrasonic 8 hours of this composite solution, under vacuum condition, remove unnecessary methyl alcohol and chloroform, with ethanol and deionized water cyclic washing three times, join subsequently in the ethanolic solution of bipyridine, refluxed 8 hours under 140 ℃ of conditions, cooling is revolved to steam and is removed unnecessary alcohol, water and ethanol washing three times, lower dry 48h obtains manocrystalline powders in 60 ℃ of baking ovens, and powder ultrasonic is distributed to deuterated dimethyl sulfoxide (DMSO), obtains transparent colloid neodymium doping gadolinium tetrafluoride natrium nanocrystalline.
Embodiment 3: the nanocrystalline (LaF of preparation transparent colloid erbium doping lanthanum fluoride
3: Er)
9 ml deionized waters, 10 ml ethanol and 20 ml (5 wt%) polymine are mixed, add the altogether rare earth nitrades (Ln (NO of 1 mmol, 0.5 mol/L to this solution under stirring
3)
3, Ln:95 mol%La, the 5mol%Er aqueous solution stirred 20 minutes, added 4 ml NH again
4F (1.0 M) aqueous solution, add subsequently 3 mol/l ammoniacal liquor to pH be 8, stirred 30 minutes.Mixed solution is transferred to 50 ml water heating kettles, in 200 ℃ of hydrothermal treatment consists 24 hours.Naturally cool off, add the cyclohexane collecting precipitation, and separate with centrifuge, wash three times with ethanol and deionized water, drying is 24 hours in 60 ℃ of baking ovens.It is nanocrystalline with the erbium doping lanthanum fluoride of polymine to obtain the surface.
With the LaF of 0.12g surface with polymine
3: Er joins the methyl alcohol of 60 ml: chloroform (1:1; v/v) in the mixed solvent; in the chloroformic solution that contains ammoniacal liquor (PH=8), slowly drip above-mentioned mixed solution; with this composite solution after ultrasonic 6 hours; under vacuum condition, remove unnecessary methyl alcohol and chloroform; with ethanol and deionized water cyclic washing three times; join subsequently in the ethanolic solution of pentanedione; refluxed 4 hours under 80 ℃ of conditions, cooling is revolved to steam and is removed unnecessary alcohol; wash three times with deionized water and ethanol; dry 48h obtains manocrystalline powders in 60 ℃ baking oven, and powder ultrasonic is distributed in the deuterated acetone, and it is nanocrystalline to obtain transparent colloid erbium doping lanthanum fluoride.
Embodiment 4: preparation transparent colloid ytterbium thulium codope tetrafluoride yttrium natrium nanocrystalline (NaYF
4: Yb/Tm)
9 ml deionized waters, 10 ml ethanol and 20 ml (5 wt%) PVP are mixed, add the altogether rare earth-iron-boron (Lncl of 1 mmol, 0.5 mol/L to this solution under stirring
3, Ln:70 mol%Gd, 28 mol%Yb, the 2 mol%Tm aqueous solution stirred 10 minutes, added 4 ml NaF (1.0 M) aqueous solution again, and adding subsequently 0.03mol/l ammoniacal liquor adjusting PH is 7, stirs 40 minutes.Mixed solution is transferred to 50 ml water heating kettles, in 220 ℃ of hydrothermal treatment consists 22 hours.Naturally cool off, add the ethanol collecting precipitation, and separate with centrifuge, wash three times with ethanol and deionized water, drying is 48 hours in 60 ℃ of baking ovens.Can obtain the surface with polyethylene pyrroles's ytterbium thulium codope tetrafluoride yttrium natrium nanocrystalline.
With the NaGdF of 0.06g surface with the polyethylene pyrroles
4: Nd joins the methyl alcohol of 60 ml: chloroform (1:1, v/v) in the mixed solvent, in the chloroformic solution that contains ammoniacal liquor (pH=10), slowly drip above-mentioned mixed solution, with this composite solution after ultrasonic 4 hours, under vacuum condition, remove unnecessary methyl alcohol and chloroform, with ethanol and deionized water cyclic washing three times, join subsequently in the benzoic ethanolic solution, refluxed 4 hours under 80 ℃ of conditions, cooling is revolved to steam and is removed unnecessary alcohol, water and ethanol washing three times, dry 48h obtains manocrystalline powders in 60 ℃ drying box, and powder ultrasonic is distributed to deuterium in the DMF; Obtain transparent colloid ytterbium thulium codope tetrafluoride yttrium natrium nanocrystalline, be prepared transparent colloid laser medium.
Below in conjunction with accompanying drawing the fluid state laser that transparent colloid laser medium of the present invention makes up is described in further detail.
Among Fig. 1, comprise diode-end-pumped source 1, first lens 2, the second lens 3, plano-concave mirror 4, the laser medium circulatory system 5, average mirror 6; The laser of described diode-end-pumped source 1 output, incide the laser medium circulatory system 5 behind the 4f system collimation that process first lens 2 and the second lens 3 form, by plano-concave mirror 4 and laserresonator that average mirror 6 forms, plano-concave mirror 4 is input mirror, average mirror 6 is outgoing mirror, and plano-concave mirror and average mirror are through coating film treatment.
Among Fig. 2, the laser medium circulatory system 5 in the described fluid state laser is comprised of laser medium fixture 7, adpting flange 8, flexible pipe 9, transparent colloid liquid reserve tank 10 and circulating pump 11; Described laser medium fixture 7 links to each other with flexible pipe 9 sealings by adpting flange 8, flexible pipe 9 is tightly connected with transparent colloid liquid reserve tank 10 1 ends, transparent colloid liquid reserve tank 10 other ends link to each other with circulating pump 11 sealings by flexible pipe, and circulating pump 11 links to each other with 7 sealings of laser medium fixture by adpting flange 8 again.
Among Fig. 3, the laser medium fixture 7 in the described laser medium circulatory system 5 is comprised of the first filming titanium jewel disk 12, the second plated film titanium jewel sheet 14, conduit 13, copper coin sheet 15 and sealing ring 16; Described the first filming titanium jewel disk 12 and the second plated film titanium jewel disk 14 separate by sealing ring 16, and it forms microcavity between the two; Described plated film titanium jewel disk 14 links to each other with 15 sealings of copper coin sheet by paraffin, and sealing links to each other another titanium jewel disk 12 with copper jewel disk by paraffin equally, and described conduit 13 joins with 15 sealings of copper coin sheet.
Claims (9)
1. the preparation method of a transparent colloid laser medium is characterized in that comprising successively following processing step:
(1) the preparation rare earth activation ion is rare earth doped nanocrystalline
In the mixed solution that contains solvent and surfactant, add rare-earth salts, stirred 10~30 minutes; Add subsequently villiaumite and get composite solution, regulate its pH value 6~9, stirred 10~60 minutes; Again composite solution is transferred in the water heating kettle, 160~230 ℃ of lower reactions 6~36 hours; Add ethanol or cyclohexane collecting precipitation, centrifugation, drying is 24 hours in 60 ℃ baking oven, and it is rare earth doped nanocrystalline namely to make rare earth activation ion;
(2) remove rare earth doped nanocrystal surface activating agent
The rare earth doped nanocrystalline concentration with 0.2g/L~2.0g/L of the rare earth activation ion that at room temperature step (1) is made is dispersed in and gets mixed solution in methyl alcohol and the chloroform, described mixed solution slowly is added drop-wise in acidity or the alkaline chloroformic solution, sonic oscillation 4~8 hours, under vacuum condition, remove unnecessary methyl alcohol and chloroform, remove the activating agent of rare earth doped nanocrystal surface;
(3) utilize the organic ligand sensitization rare earth doped nanocrystalline
Rare earth doped nanocrystallinely join sensitization in the ethanolic solution that contains organic part with what step (2) was removed surfactant, under 60~140 ℃ of temperature conditions, refluxed 2~8 hours, revolve to steam after reaction is finished and remove unnecessary alcohol;
(4) acquisition of transparent colloid laser medium
With ethanol and deionized water with the reacted rare earth doped nanocrystalline cyclic washing of step (3) three times, drying is 48 hours in 60 ℃ baking oven, again dried rare earth doped manocrystalline powders is dispersed in the organic media in heavy water or deuterium generation, namely obtains the transparent colloid laser medium.
2. preparation method according to claim 1 is characterized in that described rare-earth salts is rare earth nitrades or rare earth-iron-boron, and described villiaumite is sodium fluoride or ammonium fluoride or bifluoride hydrogen ammonia; Prepared rare earth activation ion rare earth doped nanocrystalline be the fluoride of lanthanum, cerium, praseodymium, neodymium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium; Or oxide; Or phosphate; Or vanadate, or fluoride is received salt.
3. preparation method according to claim 1 and 2 is characterized in that described rare earth activation ion is neodymium or europium or holmium or erbium or thulium or rare earth activation ion pair; Described rare earth activation ion is to being ytterbium/dysprosium or ytterbium/holmium or ytterbium/erbium or ytterbium/thulium; The percentage that described rare earth activation ion consumption accounts for total rare earth (TRE) ionic species amount is 1~25%.
4. preparation method according to claim 1; it is characterized in that described organic ligand is benzoic acid or tropolone or hexanitrodiphenyl amine or beta-diketon class, described beta-diketon class is pentanedione or Phen or bipyridine or trifluoroacetylacetone (TFA).
5. preparation method according to claim 1 is characterized in that described deuterium is that deuterated methanol or deuterated acetone or deuterium are for DMF or deuterated dimethyl sulfoxide for organic media.
6. preparation method according to claim 1 is characterized in that described solvent is deionized water, methyl alcohol or ethanol or ethylene glycol or diethylene glycol or octadecylene; Described surfactant is polymine or polyvinylpyrrolidone or polyacrylic acid or oleic acid or citric acid or ethylenediamine tetra-acetic acid or ten hexamethyl trimethylammonium bromides.
7. the fluid state laser that each prepared transparent colloid laser medium of claim 1-6 makes up is characterized in that comprising diode-end-pumped source (1), first lens (2), the second lens (3), plano-concave mirror (4), the laser medium circulatory system (5), average mirror (6); The laser of described diode-end-pumped source (1) output, incide the laser medium circulatory system (5) behind the 4f system collimation that process first lens (2) and the second lens (3) form, form laserresonator by plano-concave mirror (4) and average mirror (6), plano-concave mirror (4) is input mirror, and average mirror (6) is outgoing mirror.
8. the fluid state laser that makes up of described transparent colloid laser medium according to claim 7 is characterized in that the described laser medium circulatory system (5) is comprised of laser medium fixture (7), adpting flange (8), flexible pipe (9), transparent colloid liquid reserve tank (10) and circulating pump (11); Described laser medium fixture (7) is connected with flexible pipe (9) by adpting flange (8), flexible pipe (9) is connected with transparent colloid liquid reserve tank (10), transparent colloid liquid reserve tank (10) injects laser medium fixture (7) by circulating pump (11) with the transparent colloid in the case, and transparent colloid is circulated.
9. according to claim 7 or the fluid state laser that makes up of 8 described transparent colloid laser mediums, it is characterized in that described laser medium fixture (7) is by the first filming titanium jewel disk (12) and the second plated film titanium jewel sheet (14), conduit (13), copper coin sheet (15) and sealing ring (16) formation; The first filming titanium jewel disk (12) and the second plated film titanium jewel disk (14) separate by sealing ring (16), and it forms microcavity between the two, and conduit (9) is tightly connected with copper coin sheet (15).
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CN101935208A (en) * | 2010-08-06 | 2011-01-05 | 中国科学院理化技术研究所 | Rare earth aluminate single-phase or complex-phase nanocrystalline transparent ceramic material and preparation method thereof |
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Application publication date: 20130116 |