CN102674843B - Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof - Google Patents

Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof Download PDF

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CN102674843B
CN102674843B CN201210129953.9A CN201210129953A CN102674843B CN 102674843 B CN102674843 B CN 102674843B CN 201210129953 A CN201210129953 A CN 201210129953A CN 102674843 B CN102674843 B CN 102674843B
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梅炳初
李小女
宋京红
李威威
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Wuhan University of Technology WUT
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Abstract

The invention provides an Er3+ and Na+cadoping CaF2 transparent ceramic and a preparation method thereof. The preparation method includes: synthesis of precursor powder and sintering and post-processing of the transparent ceramic. The precursor powder is prepared by adopting a direct precipitation method in water solution, grain size of the precursor powder is 15-50nm, synthetic Er3+: CaF2 nano powder and NaF powder are mixed with alcohol fully, and Er3+, Na+: CaF2 transparent ceramic is prepared by vacuum hot-pressing sintering. Maximum transmissivity of visible light and near-infrared wave band is 85.096%, the transparent ceramic has strong absorption peak at the positions of 377nm, 519nm and 654nm and has wind absorption belt at the positions of 975nm and 1530nm, and can be used as a working gain medium for infrared and up-conversion laser. The erbium sodium codoping calcium fluoride transparent ceramic and the preparation method of the erbium sodium codoping calcium fluoride transparent ceramic are simple to operate, ceramic sintering temperature is low, ceramic sintering time is short, and the Er3+, Na+: CaF2 transparent ceramic is long in fluorescent life time.

Description

Erbium sodium is mixed Calcium Fluoride (Fluorspan) crystalline ceramics and preparation method thereof altogether
Technical field
The present invention relates to a kind of Er 3+and Na +mix altogether CaF 2crystalline ceramics and preparation method thereof, this Er 3+, Na +: CaF 2the fluorescence lifetime of crystalline ceramics is higher than singly mixing Er 3+: CaF 2crystalline ceramics, belongs to laser transparent ceramic preparing technical field.
Background technology
Er 3+the laserable material of doping all has luminous at the 1.5 μ m in safety range of human eye and two wave bands of 2.9 μ m, and the laser of this wave band can be widely used in the fields such as optical communication, medical treatment, lidar light detection and ranging very much.In addition, Er 3+, there is cross-relaxation phenomenon in some laser wavelength of ion, be particularly suitable for laser pumping under high-concentration dopant, cooperates conversion pumping, is a kind of up-conversion with broad prospect of application.
The impact of the optical property of substrate material on system is great to closing, CaF 2crystalline material is the most excellent substrate material of current known over-all properties, has numerous excellent properties compared with oxide compound: the transmission peak wavelength scope of non-constant width, cover ultraviolet in infrared region; Low phonon energy can reduce the radiationless transition probability causing because of multi-phonon relaxation greatly, makes active ions in matrix, have higher luminous quantum efficiency, is suitable as rare-earth-doped fluoride substrate material, the good optical property of performance rare earth metal.Rear-earth-doped CaF 2the research of monocrystalline laserable material has obtained gratifying achievement, the Yb of report in 2008 3+: CaF 2laser apparatus, under the pumping of 64W laser dual-laser pipe (LD), has realized average output power 10.2W, and the continuous laser that slope efficiency is 21.6% is exported (referring to document Boudeile, J.; Didierjean, J.; Camy, P.; Doualan, J. L.; Benayad, A.; M ú nard, V.; Moncorg ú, R.; Druon, F.; Balembois, F.; Georges, P., Thermal behaviour of ytterbium-doped fluorite crystals under high power pumping. Opt. Express 2008,16,10098-10109.); The people such as 2009 Nian Chai roads have successfully prepared Yb, Na and have mixed altogether CaF 2continuous wave laser obtains the maximum power continuous laser output of 14.5W in the time absorbing drawing power 18.2W, and corresponding slope efficiency is that 80%(is referring to document bavin road; Ge Wenqi; Yan Jie; Hu Minglie; Wang Qingyue; Su Liangbi; Li Hongjun; Zheng Li and; Xu Jun, the ytterbium sodium of high powerdiode pumped is mixed Calcium Fluoride (Fluorspan) continuous wave laser altogether. Chinese laser 2009,36,1700.).
Rear-earth-doped CaF 2the broad research of monocrystalline is rear-earth-doped CaF 2upsurge has been pushed in the research of crystalline ceramics to.For crystal, crystalline ceramics can be realized the high-concentration dopant of active ions, and product size pattern is easy to control, and sintering temperature is low, and the production cycle shortens greatly, is easy to scale operation thereby reduce costs.But, in pottery, exist the factor such as imperfect of crystal boundary, pore, component gradient and lattice to make that the light scattering loss of material increases, light transmission reduces, so about doping CaF 2the report of crystalline ceramics is little, Bensalah in 2006, and A etc. have reported and have synthesized the CaF that median size is 20nm by reverse microemulsion process 2nano-powder, for next step ceramic post sintering has been laid a foundation basis (referring to document Bensalah, A.; Mortier, M.; Patriarche, G.; Gredin, P.; Vivien, D., Synthesis and optical characterizations of undoped and rare-earth-doped CaF 2nanoparticles. J. Solid State Chem. 2006,179,2636-2644.), 2009 Aubry, the people such as P have successfully prepared Yb:CaF 2crystalline ceramics, and its optical property is characterized (referring to document Aubry, P.; Bensalah, A.; Gredin, P.; Patriarche, G.; Vivien, D.; Mortier, M., Synthesis and optical characterizations of Yb-doped CaF 2ceramics. Opt. Mater. 2009,31,750-753.).
Along with the development of technology of preparing and the high-vacuum sintering technique of nano-powder, Re:CaF 2crystalline ceramics, due to its good optical property, thermomechanical property and stable physico-chemical property, is expected to replace Re:CaF 2monocrystalline, has caused numerous experts and scholars' very big concern.Adopt suitable nano material synthetic technology to prepare high purity, good dispersity, particle size dispersion even, there is higher sintering activity, be conducive to prepare high-quality crystalline ceramics.
summary of the invention
Main purpose of the present invention is to provide one and mixes altogether sodium and erbium Calcium Fluoride (Fluorspan) crystalline ceramics and preparation method thereof, to improve Er:CaF 2the fluorescence lifetime of crystalline ceramics.
Technical solution of the present invention is as follows:
Erbium sodium is mixed a preparation method for Calcium Fluoride (Fluorspan) crystalline ceramics altogether, comprises the sintering of the synthetic and crystalline ceramics of sintering powder, and preparation process is as follows:
1) sintering powder is synthetic:
With the Ca (NO of purity>=99.0% 3) 24H 2o, the Er (NO of purity>=99.99% 3) 35H 2o, the KF2H of purity>=99.0% 2o is raw material, adopts direct precipitation method in the aqueous solution to generate Er 3+: CaF 2nanoparticle suspension, by gained Er 3+: CaF 2nanoparticle suspension is placed on 60～120 DEG C of vacuum-dryings for three times by deionized water wash, centrifugation, obtains Er 3+: CaF 2nanometer powder;
By the Er obtaining 3+: CaF 2nanometer powder in 60～120 DEG C of vacuum-dryings, obtains sintering powder after fully mixing in alcohol with NaF powder;
2) sintering of crystalline ceramics:
The sintering powder of preparing in step 1) being packed in graphite jig, be then placed in vacuum hotpressing stove, is sintering under 500～1000 DEG C, pressure 10～60MPa, the processing condition of 30～180 minutes heat-insulation pressure keeping time in sintering temperature;
3) aftertreatment:
By step 2) sample after sintering takes out, and adopts after sand paper corase grind, and on UNIPOL-802 type precise grinding polisher, after twin polishing, obtain erbium sodium and mix altogether Calcium Fluoride (Fluorspan) crystalline ceramics finished product.
In preparation method's step 1) of the present invention, synthetic Er 3+: CaF 2nanometer powder process is first to weigh Ca (NO 3) 24H 2o, Er (NO 3) 35H 2o and KF2H 2o, is dissolved in respectively in deionized water, is mixed with the Ca that volumetric molar concentration is 0.25～10mol/L 2+and Er 3+cationic solution and volumetric molar concentration are the F of 0.5～20mol/L -anion solutions, Ca in cationic solution 2+and Er 3+molar content is than being n(Ca 2+): n(Er 3+)=99:1～90:10), then by the rapid hybrid reaction of two solution.
In preparation method's step 1) of the present invention, the Er of preparation 3+: CaF 2the grain-size of nanometer powder is 15～50nm.
In preparation method's step 1) of the present invention, Er 3+: CaF 2in nanometer powder and NaF powdered mixture, Na +the content of ion is 0.5mol%～1.5mol%.
Preparation method's step 2 of the present invention) in, the vacuum hotpressing stove of crystalline ceramics sintering is the KZG-113 type vacuum hotpressing stove that Shanghai Chen Rong electric furnace company limited produces, and temperature rise rate is 8～50 DEG C/min, and cooling is furnace cooling.
The grain-size that the prepared erbium sodium of method of the present invention is mixed Calcium Fluoride (Fluorspan) crystalline ceramics is altogether 200～500nm, density >=99.7, at the maximum transmission 85.096% of visible ray, near-infrared band, the fluorescence lifetime that the erbium sodium of preparation is mixed Calcium Fluoride (Fluorspan) crystalline ceramics altogether reaches most 10.74ms.
The present invention compared with prior art has advantages of following main:
1, adopt Direct precipitation legal system agglomerated powder body, there is the advantages such as technique is simple, easy and simple to handle, not high and output is large to equipment requirements.
2, adopt vacuum hot pressing sintering technique to prepare Er 3+, Na +: CaF 2crystalline ceramics, in vacuum environment, avoid ceramic oxidation, heat simultaneously, pressurize, the mass transfer process such as contribute to the contact, diffusion of powder particle and flow, reduce sintering temperature and shorten sintering time, easy acquisition approaches theoretical density and void content approaches zero sintered compact, obtains the good product of mechanical property and photoelectric properties.
3. at CaF 2in matrix, enter Er simultaneously 3+and Na +, Er 3+and Na +replacing Ca 2+time form electric charge complementation to reach charge balance, stop Er simultaneously 3+the formation of ionic group clustering architecture, improves Er greatly 3+, Na +: CaF 2the fluorescence lifetime of crystalline ceramics.
The present invention is that erbium sodium is mixed Calcium Fluoride (Fluorspan) crystalline ceramics altogether, and this pottery has high transmittance and long fluorescence lifetime, can be used for developing high efficiency LD light-pumped solid state laser dielectric material.
brief description of the drawings
Fig. 1 is Er 3+(5 mol %), Na +(1 mol %): CaF 2crystalline ceramics schematic diagram, sample size is diameter 16mm, can be clearly seen that word below by sample, the transparency is good;
Fig. 2 is Er 3+(5 mol %), Na +(1 mol %): CaF 2the transmittance curve figure of crystalline ceramics, the ceramic transmitance that shows transparency in figure is higher, the maximum transmission 85.096% of wave band outside visible ray, near infrared, there is stronger absorption peak at 377nm, 519nm and 654nm place, there is wider absorption band at 975nm and 1530nm place, can be used as infrared and up-conversion lasing working gain medium;
Figure 3 shows that the Er recording under the same terms 3+, Na +: CaF 2and Er 3+: CaF 2crystalline ceramics is at 978nmLD
Excite lower 1530nm fluorescence intensity extinction curve in time;
Curve (a) represents singly to mix Er 3+(5 mol %): CaF 2crystalline ceramics;
Curve (b) represents Er 3+(5 mol %), Na +(0.5 mol %): CaF 2crystalline ceramics;
Curve (c) represents Er 3+(5 mol %), Na +(1.0 mol %): CaF 2crystalline ceramics;
Curve (d) represents Er 3+(5 mol %), Na +(1.5 mol %): CaF 2crystalline ceramics .
embodiment
Below by embodiment, the present invention is further described, but should not limit the scope of the invention with this.Embodiment is with the Ca (NO of purity>=99.0% 3) 24H 2o, the Er (NO of purity>=99.99% 3) 35H 2o, the KF2H of purity>=99.0% 2o is raw material.
Embodiment 1
Take Ca (NO 3) 24H 2o, Er (NO 3) 35H 2o and KF2H 2o, is dissolved in respectively in deionized water, is mixed with the Ca that volumetric molar concentration is 0.5mol/L 2+and Er 3+cationic solution, the F that volumetric molar concentration is 0.5mol/L -anion solutions, Ca in cationic solution 2+and Er 3+molar content than for n(Ca 2+): n(Er 3+)=95:5, then by the rapid hybrid reaction of two solution.By gained Er 3+: CaF 2nanoparticle suspension is placed on 75 DEG C of vacuum-dryings for three times by deionized water wash, centrifugation, obtains the Er that grain-size is 15～50nm 3+: CaF 2nanometer powder.Er will singly be mixed 3+: CaF 2nanometer powder packs in graphite jig, sintering in vacuum hotpressing stove, and temperature rise rate is 15 DEG C/min, 800 DEG C of sintering temperatures, pressure 30MPa, 60 minutes heat-insulation pressure keeping time, cooling is furnace cooling.
Gained sample is after the sand paper corase grind of different model, on UNIPOL-802 type precise grinding polisher, after twin polishing, obtain erbium doping Calcium Fluoride (Fluorspan) crystalline ceramics finished product, density 99.8%, adopt the transmitance of UV3600 type ultraviolet-visible-near infrared spectrometer test sample of Japanese Shimadzu company, it is that the transmitance at 1363nm place is 80.453% that result is presented at wavelength.Adopt TektronixTDS3012 digital oscilloscope to be recorded in luminous intensity that 978nmLD excites lower 1530nm over time, as shown in (a) curve in Fig. 3, adopt first-order exponential decay function (y=A1*exp(-x/t 1)+y 0) matching actual measurement extinction curve, the fluorescence lifetime calculating is 5.55ms.
Embodiment 2
Er 3+blended amount is the Er of 5mol% 3+: CaF 2the preparation of nanometer powder is identical with embodiment 1 method, by the Er of gained 3+: CaF 2nanometer powder and NaF powder (Na +ion content is 0.5mol%) in alcohol, fully mix, then dry and be sintering powder.By sintering powder sintering in vacuum hotpressing stove, processing parameter is as identical in embodiment 1.
After the twin polishing of gained sample, obtain erbium sodium and mix altogether Calcium Fluoride (Fluorspan) crystalline ceramics finished product, density 99.9%, the transmitance that is 1363nm place at wavelength is 83.998%.Over time, as shown in (b) curve in Fig. 3, simulate fluorescence lifetime is 5.91ms to the luminous intensity that excites lower 1530nm at 978nmLD.
Embodiment 3
Er 3+blended amount is the Er of 5mol% 3+: CaF 2the preparation of nanometer powder is identical with embodiment 1 method, by the Er of gained 3+: CaF 2nanometer powder and NaF powder (Na +ion content is 1.0mol%) in alcohol, fully mix, then dry and be sintering powder.By sintering powder sintering in vacuum hotpressing stove, processing parameter is as identical in embodiment 1.
Gained sample obtains erbium sodium and mixes altogether Calcium Fluoride (Fluorspan) crystalline ceramics finished product as shown in Figure 1 after twin polishing, density 99.94%, the transmitance that adopts UV3600 ultraviolet-visible-near infrared spectrometer test sample of Japanese Shimadzu company, result as shown in Figure 2.The transmitance that is 1363nm place at wavelength is 85.096%.Over time, as shown in (c) curve in Fig. 3, simulate fluorescence lifetime is 7.13ms to the luminous intensity that excites lower 1530nm at 978nmLD.
As can be seen from the figure along with Na +the increase of incorporation, the fluorescence lifetime of crystalline ceramics significantly increases.
Embodiment 4
Er 3+blended amount is the Er of 5mol% 3+: CaF 2the preparation of nanometer powder and embodiment 1 method use mutually, by the Er of gained 3+: CaF 2nanometer powder and NaF powder (Na +ion content is 1.5mol%) in alcohol, fully mix, then dry and be sintering powder.By sintering powder sintering in vacuum hotpressing stove, processing parameter is identical as described in Example 1.
Gained sample obtains erbium sodium and mixes altogether Calcium Fluoride (Fluorspan) crystalline ceramics finished product after twin polishing, density 99.91%, the transmitance that is 1363nm place at wavelength is 84.784%, the luminous intensity that excites lower 1530nm at 978nmLD over time, as shown in (b) curve in Fig. 3, simulating fluorescence lifetime is 6.38ms.Draw and mix altogether Na +the fluorescence lifetime that ion improves crystalline ceramics should have individual optimum value.
Embodiment 5
Weigh Ca (NO according to stoichiometric ratio 3) 24H 2o, Er (NO 3) 35H 2o and KF2H 2o, is dissolved in respectively in deionized water, is configured to the Ca that volumetric molar concentration is 0.5mol/L 2+and Er 3+cationic solution and volumetric molar concentration are the F of 0.5mol/L -anion solutions, Ca 2+and Er 3+cationic solution in, Ca 2+and Er 3+molar content than for n(Ca 2+): n(Er 3+)=99:1, then by the rapid hybrid reaction of two solution.By gained Er 3+: CaF 2nanoparticle suspension is placed on 75 DEG C of vacuum-dryings for three times by deionized water wash, centrifugation, and obtaining grain-size is 15-50nm, Er 3+: CaF 2nanometer powder.Er will singly be mixed 3+(1mol%): CaF 2nanometer powder is sintering in vacuum hotpressing stove, and processing parameter as described in Example 1.
Gained sample obtains er-doped Calcium Fluoride (Fluorspan) crystalline ceramics finished product after twin polishing, density 99.7%, the transmitance that is 1363nm place at wavelength is 76.453%, the luminous intensity that excites lower 1530nm at 978nmLD over time, matching actual measurement extinction curve, the fluorescence lifetime calculating is 4.91ms.
Embodiment 6
Er 3+(1mol%): CaF 2the preparation of nanometer powder is identical with embodiment 5 methods, by the Er of gained 3+: CaF 2nanometer powder and NaF powder (Na +ion content is 1.0mol%) in alcohol, fully mix, then dry and be sintering powder.By sintering powder sintering in vacuum hotpressing stove, processing parameter as described in Example 1.
Gained sample obtains erbium sodium and mixes altogether Calcium Fluoride (Fluorspan) crystalline ceramics finished product after twin polishing, density 99.76%, the transmitance that is 1363nm place at wavelength is 84.784%, the luminous intensity that excites lower 1530nm at 978nmLD over time, matching actual measurement extinction curve, the fluorescence lifetime calculating is 10.74ms.
In order to make entire article brief introduction, only enumerate 6 specific embodiments of the present invention above, experiment showed, by the range of choice of the present invention program's raw material and condition, can prepare well behaved erbium sodium and mix altogether Calcium Fluoride (Fluorspan) crystalline ceramics.

Claims (5)

1. erbium sodium is mixed a preparation method for Calcium Fluoride (Fluorspan) crystalline ceramics altogether, it is characterized in that, comprises the sintering of the synthetic and crystalline ceramics of sintering powder, and preparation process is as follows:
1) sintering powder is synthetic:
With the Ca (NO of purity>=99.0% 3) 24H 2o, the Er (NO of purity>=99.99% 3) 35H 2o, the KF2H of purity>=99.0% 2o is raw material, adopts direct precipitation method in the aqueous solution to generate Er 3+: CaF 2nanoparticle suspension, by gained Er 3+: CaF 2nanoparticle suspension is placed on 60～120 DEG C of vacuum-dryings for three times by deionized water wash, centrifugation, obtains Er 3+: CaF 2nanometer powder, described synthetic Er 3+: CaF 2in nanometer powder process, first weigh Ca (NO 3) 24H 2o, Er (NO 3) 35H 2o and KF2H 2o, is dissolved in respectively in deionized water, is mixed with the Ca that volumetric molar concentration is 0.25～10mol/L 2+and Er 3+cationic solution and volumetric molar concentration are the F of 0.5～20mol/L -anion solutions, Ca in cationic solution 2+and Er 3+molar content is than being n(Ca 2+): n(Er 3+)=99:1～90:10, then by the rapid hybrid reaction of two solution;
By the Er obtaining 3+: CaF 2nanometer powder in 60～120 DEG C of vacuum-dryings, obtains sintering powder, described Er after fully mixing in alcohol with the NaF powder of purity>=99.0% 3+: CaF 2in nanometer powder and NaF powdered mixture, Na +the content of ion is 0.5mol%～1.5mol%;
2) sintering of crystalline ceramics:
The sintering powder of preparing in step 1) being packed in graphite jig, be then placed in vacuum hotpressing stove, is sintering under 500～1000 DEG C, pressure 10～60MPa, the processing condition of 30～180 minutes heat-insulation pressure keeping time in sintering temperature;
3) aftertreatment:
By step 2) sample after sintering takes out, and adopts after sand paper corase grind, and on UNIPOL-802 type precise grinding polisher, after twin polishing, obtain erbium sodium and mix altogether Calcium Fluoride (Fluorspan) crystalline ceramics finished product.
2. the preparation method who mixes altogether Calcium Fluoride (Fluorspan) crystalline ceramics by erbium sodium claimed in claim 1, is characterized in that, during sintering powder described in step 1) is synthetic, and the Er of preparation 3+: CaF 2the grain-size of nanometer powder is 15～50nm.
3. the preparation method who mixes altogether Calcium Fluoride (Fluorspan) crystalline ceramics by erbium sodium claimed in claim 1, it is characterized in that step 2) in crystalline ceramics sintering, vacuum hotpressing stove is the KZG-113 type vacuum hotpressing stove that Shanghai Chen Rong electric furnace company limited produces, temperature rise rate is 8～50 DEG C/min, and cooling is furnace cooling.
4. the preparation method who mixes altogether Calcium Fluoride (Fluorspan) crystalline ceramics by erbium sodium claimed in claim 1, it is characterized in that, the grain-size that prepared erbium sodium is mixed Calcium Fluoride (Fluorspan) crystalline ceramics is altogether 200～500nm, and density >=99.7 are 85.096% at the maximum transmission of visible ray and near-infrared band.
5. the preparation method who mixes altogether Calcium Fluoride (Fluorspan) crystalline ceramics by erbium sodium claimed in claim 1, is characterized in that, the fluorescence lifetime that prepared erbium sodium is mixed Calcium Fluoride (Fluorspan) crystalline ceramics altogether reaches most 10.74ms.
CN201210129953.9A 2012-04-28 2012-04-28 Erbium sodium codoping calcium fluoride transparent ceramic and preparation method thereof Expired - Fee Related CN102674843B (en)

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EP2927202A1 (en) * 2014-04-04 2015-10-07 Paris Sciences et Lettres - Quartier Latin Transparent metal fluoride ceramic
EP3208253A1 (en) 2016-02-16 2017-08-23 Centre National De La Recherche Scientifique Transparent fluoride ceramic material and a method for its preparation
CN105948751B (en) * 2016-04-21 2018-11-13 武汉理工大学 Neodymium adulterates strontium fluoride laser transparent ceramic and preparation method thereof
CN106220179A (en) * 2016-07-10 2016-12-14 九江学院 A kind of Ba2laF7: Er3+the preparation method of upper conversion transparent ceramic
CN107628813B (en) * 2017-09-25 2020-05-22 信阳师范学院 Method for reducing sintering temperature of polycrystalline transparent ceramic prepared from fluorite mineral
CN107619280B (en) * 2017-10-12 2021-01-15 信阳师范学院 Preparation method of layered calcium fluoride transparent ceramic
CN108640686B (en) * 2018-06-27 2021-03-16 武汉理工大学 Europium-yttrium co-doped calcium fluoride scintillating ceramic and preparation method thereof

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