CN102674843A - 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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CN102674843A
CN102674843A CN2012101299539A CN201210129953A CN102674843A CN 102674843 A CN102674843 A CN 102674843A CN 2012101299539 A CN2012101299539 A CN 2012101299539A CN 201210129953 A CN201210129953 A CN 201210129953A CN 102674843 A CN102674843 A CN 102674843A
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sintering
crystalline ceramics
preparation
calcium fluoride
caf
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CN102674843B (en
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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 CaF altogether 2Crystalline ceramics and preparation method thereof, this Er 3+, Na +: CaF 2The fluorescence lifetime of crystalline ceramics is higher than singly mixes Er 3+: CaF 2Crystalline ceramics belongs to the laser transparent ceramic preparing technical field.
Background technology
Er 3+Adulterated laserable material all has luminous at the 1.5 μ m that are 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 fields such as optical communication, medical treatment, lidar very much.In addition, Er 3+There is the cross-relaxation phenomenon in some laser wavelength of ionic under high-concentration dopant, be particularly suitable for laser pumping, promptly cooperates the conversion pumping, is a kind of up-conversion with broad prospect of application.
Substrate material is great to closing to the influence of the optical property of system, CaF 2Crystalline material is the most excellent substrate material of present known over-all properties, compares with oxide compound to have numerous excellent properties: the transmission peak wavelength scope of non-constant width, cover ultraviolet in infrared zone; Low phonon energy can reduce the radiationless transition probability that causes because of the multi-phonon relaxation greatly, makes active ions in matrix, have higher luminous quantum efficiency, is suitable as the rare-earth-doped fluoride substrate material, performance rare earth metal good optical performance.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 been realized average output power 10.2W, and slope efficiency is that the output of 21.6% continuous laser is (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.); People such as Chai Lu in 2009 have successfully prepared Yb, Na and have mixed CaF altogether 2Continuous wave laser obtains the maximum power continuous laser output of 14.5W when absorbing drawing power 18.2W, corresponding slope efficiency is 80% (referring to document bavin road; Ge Wenqi; Yan Jie; Hu Minglie; Wang Qingyue; Su Liangbi; Li Hongjun; Zheng Li with; Xu Jun, the ytterbium sodium of high-power laser diode pumping is mixed the 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 the 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 cost.But, exist the factor such as imperfect of crystal boundary, pore, component gradient and lattice to make that the scattering of light loss of material increases, light transmission reduces in the pottery, so about doping CaF 2The report of crystalline ceramics seldom, Bensalah in 2006, A etc. have reported and have used reverse microemulsion process to synthesize the CaF of median size as 20nm 2Nano-powder is for next step ceramic post sintering has been laid a foundation the 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, people such as P have successfully prepared Yb:CaF 2Crystalline ceramics, and its optical property 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 technology of preparing of nano-powder and the development of high vacuum sintering process, Re:CaF 2Crystalline ceramics is because its good optical performance, thermomechanical property and stable physico-chemical property are expected to replace Re:CaF 2Monocrystalline has caused numerous experts and scholars' very big concern.It is even to adopt suitable nano material synthetic technology to prepare high purity, good dispersivity, particle size dispersion, has higher sintering activity, helps preparing high-quality crystalline ceramics.
Summary of the invention
Main purpose of the present invention provides a kind of sodium and erbium Calcium Fluoride (Fluorspan) crystalline ceramics and preparation method thereof mixed altogether, to improve Er:CaF 2The fluorescence lifetime of crystalline ceramics.
Technical solution of the present invention is following:
A kind of erbium sodium is mixed the preparation method of Calcium Fluoride (Fluorspan) crystalline ceramics altogether, comprises the sintering of the synthetic and crystalline ceramics of sintering powder, and preparation process is following:
1) the sintering powder is synthetic:
Ca (NO with purity>=99.0% 3) 24H 2O, the Er (NO of purity>=99.99% 3) 35H 2O, the KF2H of purity>=99.0% 2O is a raw material, adopts direct precipitation method generation Er in the aqueous solution 3+: CaF 2Nanoparticle suspension is with gained Er 3+: CaF 2Nanoparticle suspension is placed on 60～120 ℃ of vacuum-dryings for three times through deionized water wash, spinning, obtains Er 3+: CaF 2Nanometer powder;
With the Er that obtains 3+: CaF 2Nanometer powder and NaF powder behind the thorough mixing, in 60～120 ℃ of vacuum-dryings, obtain the sintering powder in alcohol;
2) sintering of crystalline ceramics:
The sintering powder for preparing in the step 1) being packed in the graphite jig, be placed on then in the vacuum hotpressing stove, is sintering under 500～1000 ℃, pressure 10～60MPa, the processing condition of 30～180 minutes heat-insulation pressure keeping time in sintering temperature;
3) aftertreatment:
With step 2) sample behind the sintering takes out, adopt the sand paper corase grind after, after twin polishing on the UNIPOL-802 type precise grinding polisher, obtain erbium sodium and mix Calcium Fluoride (Fluorspan) crystalline ceramics finished product altogether.
In preparing method's step 1) of the present invention, synthetic Er 3+: CaF 2The nanometer powder process is first weighing Ca (NO 3) 24H 2O, Er (NO 3) 35H 2O and KF2H 2O is dissolved in respectively in the 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 the cationic solution 2+And Er 3+Molar content is than being n (Ca 2+): n (Er 3+)=99:1～90:10), then with the rapid hybrid reaction of two solution.
In preparing method's step 1) of the present invention, the Er of preparation 3+: CaF 2The grain-size of nanometer powder is 15～50nm.
In preparing method's step 1) of the present invention, Er 3+: CaF 2In nanometer powder and the NaF powdered mixture, Na +Ionic content is 0.5mol%～1.5mol%.
Preparing 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 the flourish electric furnace of Shanghai occasion ltd produces, and temperature rise rate is 8～50 ℃/min, and cooling is a furnace cooling.
The grain-size that the prepared erbium sodium of method of the present invention is mixed the Calcium Fluoride (Fluorspan) crystalline ceramics altogether is 200～500nm; Density >=99.7; At the maximum transmission 85.096% of visible light, near-infrared band, the fluorescence lifetime that the erbium sodium of preparation is mixed the Calcium Fluoride (Fluorspan) crystalline ceramics altogether reaches most 10.74ms.
The present invention compared with prior art has following main advantage:
1, adopt direct precipitation method system sintering powder, have advantages such as technology is simple, easy and simple to handle, not high and output is big to equipment requirements.
2, adopt vacuum hot pressing sintering technique to prepare Er 3+, Na +: CaF 2Crystalline ceramics; In vacuum environment, avoided ceramic oxidation; Heat simultaneously, pressurize, mass transfer process such as help the contact, diffusion of powder particle and flow reduces sintering temperature and shortens sintering time; Obtain easily to obtain the good product of mechanical property and photoelectric properties near theoretical density and approaching zero the sintered compact of void content.
3. at CaF 2Get into Er in the matrix simultaneously 3+And Na +, Er 3+And Na +Replacing Ca 2+The time form the 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 the 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.
Description of drawings
Fig. 1 is Er 3+(5 mol %), Na +(1 mol %): CaF 2Crystalline ceramics synoptic diagram, sample size are diameter 16mm, can be clearly seen that following literal through sample, and 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 among the figure is higher; The maximum transmission 85.096% of wave band outside visible light, near infrared; Have stronger absorption peak at 377nm, 519nm and 654nm place, have the absorption band of broad at 975nm and 1530nm place, can be used as infrared and up-conversion lasing working gain medium;
Er for recording under the same terms shown in Figure 3 3+, Na +: CaF 2And Er 3+: CaF 2Crystalline ceramics is at 978nmLD
Excite down 1530nm fluorescence intensity extinction curve in time;
Er is singly mixed in curve (a) expression 3+(5 mol %): CaF 2Crystalline ceramics;
Curve (b) expression Er 3+(5 mol %), Na +(0.5 mol %): CaF 2Crystalline ceramics;
Curve (c) expression Er 3+(5 mol %), Na +(1.0 mol %): CaF 2Crystalline ceramics;
Curve (d) expression Er 3+(5 mol %), Na +(1.5 mol %): CaF 2Crystalline ceramics
Embodiment
Through embodiment the present invention is further specified below, but should not limit protection scope of the present 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 a raw material.
Embodiment 1
Take by weighing Ca (NO 3) 24H 2O, Er (NO 3) 35H 2O and KF2H 2O is dissolved in respectively in the deionized water, is mixed with the Ca that volumetric molar concentration is 0.5mol/L 2+And Er 3+Cationic solution, volumetric molar concentration is the F of 0.5mol/L -Anion solutions, Ca in the cationic solution 2+And Er 3+Molar content than for n (Ca 2+): n (Er 3+)=95:5 is then with the rapid hybrid reaction of two solution.With gained Er 3+: CaF 2Nanoparticle suspension is placed on 75 ℃ of vacuum-dryings for three times through deionized water wash, spinning, obtains the Er that grain-size is 15～50nm 3+: CaF 2Nanometer powder.With singly mixing Er 3+: CaF 2Nanometer powder is packed in the graphite jig, and sintering in vacuum hotpressing stove, temperature rise rate are 15 ℃/min, and 800 ℃ of sintering temperatures, pressure 30MPa, 60 minutes heat-insulation pressure keeping time, cooling is a furnace cooling.
After the sand paper corase grind of gained sample through different model; After twin polishing on the UNIPOL-802 type precise grinding polisher, obtain erbium doping Calcium Fluoride (Fluorspan) crystalline ceramics finished product; Density 99.8%; Adopt the transmitance of the UV3600 type ultraviolet-visible-near infrared spectrometer specimen of Japanese Shimadzu company, it is that the transmitance at 1363nm place is 80.453% that the result is presented at wavelength.Adopt the TektronixTDS3012 digital oscilloscope to be recorded in luminous intensity that 978nmLD excites down 1530nm over time, shown in (a) curve among Fig. 3, employing single order decaying exponential function (y=A1*exp (x/t 1)+y 0) match actual measurement extinction curve, the fluorescence lifetime that calculates 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, with the Er of gained 3+: CaF 2Nanometer powder and NaF powder (Na +Ion content is 0.5mol%) thorough mixing in alcohol, oven dry is the sintering powder then.With sintering powder sintering in vacuum hotpressing stove, processing parameter such as embodiment 1 are identical.
Obtain erbium sodium after the twin polishing of gained sample and mix Calcium Fluoride (Fluorspan) crystalline ceramics finished product altogether, density 99.9% is that the transmitance at 1363nm place is 83.998% at wavelength.The luminous intensity that excites following 1530nm at 978nmLD over time, shown in (b) curve among Fig. 3, simulating fluorescence lifetime is 5.91ms.
Embodiment 3
Er 3+Blended amount is the Er of 5mol% 3+: CaF 2The preparation of nanometer powder is identical with embodiment 1 method, with the Er of gained 3+: CaF 2Nanometer powder and NaF powder (Na +Ion content is 1.0mol%) thorough mixing in alcohol, oven dry is the sintering powder then.With sintering powder sintering in vacuum hotpressing stove, processing parameter such as embodiment 1 are identical.
To mix Calcium Fluoride (Fluorspan) crystalline ceramics finished product altogether as shown in Figure 1 through obtaining erbium sodium after the twin polishing for the gained sample; Density 99.94%; Adopt the transmitance of the UV3600 ultraviolet-visible-near infrared spectrometer specimen of Japanese Shimadzu company, the result is as shown in Figure 2.At wavelength is that the transmitance at 1363nm place is 85.096%.The luminous intensity that excites following 1530nm at 978nmLD over time, shown in (c) curve among Fig. 3, simulating fluorescence lifetime is 7.13ms.
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 be usefulness mutually, with the Er of gained 3+: CaF 2Nanometer powder and NaF powder (Na +Ion content is 1.5mol%) thorough mixing in alcohol, oven dry is the sintering powder then.With sintering powder sintering in vacuum hotpressing stove, processing parameter such as embodiment 1 are said identical.
The gained sample is mixed Calcium Fluoride (Fluorspan) crystalline ceramics finished product altogether through obtaining erbium sodium after the twin polishing; Density 99.91%; At wavelength is that the transmitance at 1363nm place is 84.784%; The luminous intensity that excites following 1530nm at 978nmLD over time, shown in (b) curve among Fig. 3, simulating fluorescence lifetime is 6.38ms.Draw and mix Na altogether +The fluorescence lifetime that ion improves crystalline ceramics should have individual optimum value.
Embodiment 5
According to stoichiometric ratio weighing Ca (NO 3) 24H 2O, Er (NO 3) 35H 2O and KF2H 2O is dissolved in respectively in the 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 is then with the rapid hybrid reaction of two solution.With gained Er 3+: CaF 2Nanoparticle suspension is placed on 75 ℃ of vacuum-dryings for three times through deionized water wash, spinning, and obtaining grain-size is 15-50nm, Er 3+: CaF 2Nanometer powder.With singly mixing Er 3+(1mol%): CaF 2Nanometer powder is sintering in vacuum hotpressing stove, and processing parameter such as embodiment 1 are said.
The gained sample obtains er-doped Calcium Fluoride (Fluorspan) crystalline ceramics finished product through after the twin polishing; Density 99.7%; At wavelength is that the transmitance at 1363nm place is 76.453%; The luminous intensity that excites following 1530nm at 978nmLD over time, match actual measurement extinction curve, the fluorescence lifetime that calculates is 4.91ms.
Embodiment 6
Er 3+(1mol%): CaF 2The preparation of nanometer powder is identical with embodiment 5 methods, with the Er of gained 3+: CaF 2Nanometer powder and NaF powder (Na +Ion content is 1.0mol%) thorough mixing in alcohol, oven dry is the sintering powder then.With sintering powder sintering in vacuum hotpressing stove, processing parameter such as embodiment 1 are said.
The gained sample is mixed Calcium Fluoride (Fluorspan) crystalline ceramics finished product altogether through obtaining erbium sodium after the twin polishing; Density 99.76%; At wavelength is that the transmitance at 1363nm place is 84.784%; The luminous intensity that excites following 1530nm at 978nmLD over time, match actual measurement extinction curve, the fluorescence lifetime that calculates is 10.74ms.
In order to make the entire article brief introduction, more than only enumerated 6 specific embodiments of the present invention, experiment showed, by the present invention program's the raw material and the range of choice of condition, can prepare well behaved erbium sodium and mix the Calcium Fluoride (Fluorspan) crystalline ceramics altogether.

Claims (7)

1. the preparation method that erbium sodium is mixed the Calcium Fluoride (Fluorspan) crystalline ceramics altogether is characterized in that, comprises the sintering of the synthetic and crystalline ceramics of sintering powder, and preparation process is following:
1) the sintering powder is synthetic:
Ca (NO with purity>=99.0% 3) 24H 2O, the Er (NO of purity>=99.99% 3) 35H 2O, the KF2H of purity>=99.0% 2O is a raw material, adopts direct precipitation method generation Er in the aqueous solution 3+: CaF 2Nanoparticle suspension is with gained Er 3+: CaF 2Nanoparticle suspension is placed on 60～120 ℃ of vacuum-dryings for three times through deionized water wash, spinning, obtains Er 3+: CaF 2Nanometer powder;
With the Er that obtains 3+: CaF 2Nanometer powder and NaF (purity>=99.0%) powder behind the thorough mixing, in 60～120 ℃ of vacuum-dryings, obtains the sintering powder in alcohol;
2) sintering of crystalline ceramics:
The sintering powder for preparing in the step 1) being packed in the graphite jig, be placed on then in the vacuum hotpressing stove, is sintering under 500～1000 ℃, pressure 10～60MPa, the processing condition of 30～180 minutes heat-insulation pressure keeping time in sintering temperature;
3) aftertreatment:
With step 2) sample behind the sintering takes out, adopt the sand paper corase grind after, after twin polishing on the UNIPOL-802 type precise grinding polisher, obtain erbium sodium and mix Calcium Fluoride (Fluorspan) crystalline ceramics finished product altogether.
2. the preparation method who mixes the Calcium Fluoride (Fluorspan) crystalline ceramics altogether by the described erbium sodium of claim 1 is characterized in that step 1) is synthesized Er 3+: CaF 2In the nanometer powder process, first weighing Ca (NO 3) 24H 2O, Er (NO 3) 35H 2O and KF2H 2O is dissolved in respectively in the 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 the cationic solution 2+And Er 3+Molar content is than being n (Ca 2+): n (Er 3+)=99:1～90:10 is then with the rapid hybrid reaction of two solution.
3. the preparation method who mixes the Calcium Fluoride (Fluorspan) crystalline ceramics altogether by the described erbium sodium of claim 1 is characterized in that, during the described sintering powder of step 1) is synthetic, and the Er of preparation 3+: CaF 2The grain-size of nanometer powder is 15～50nm.
4. the preparation method who mixes the Calcium Fluoride (Fluorspan) crystalline ceramics altogether by the described erbium sodium of claim 1 is characterized in that step 1) Er 3+: CaF 2In nanometer powder and the NaF powdered mixture, Na +Ionic content is 0.5mol%～1.5mol%.
5. the preparation method who mixes the Calcium Fluoride (Fluorspan) crystalline ceramics altogether by the described erbium sodium of claim 1; It is characterized in that step 2) in the crystalline ceramics sintering, vacuum hotpressing stove is the KZG-113 type vacuum hotpressing stove that the flourish electric furnace of Shanghai occasion ltd produces; Temperature rise rate is 8～50 ℃/min, and cooling is a furnace cooling.
6. the preparation method who mixes the Calcium Fluoride (Fluorspan) crystalline ceramics altogether by the described erbium sodium of claim 1; It is characterized in that; The grain-size that prepared erbium sodium is mixed the Calcium Fluoride (Fluorspan) crystalline ceramics altogether is 200～500nm, and density >=99.7 are 85.096% at the maximum transmission of visible light, near-infrared band.
7. the preparation method who mixes the Calcium Fluoride (Fluorspan) crystalline ceramics altogether by the described erbium sodium of claim 1 is characterized in that the fluorescence lifetime that prepared erbium sodium is mixed the Calcium Fluoride (Fluorspan) crystalline ceramics altogether reaches most 10.74ms.
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EP2927202A1 (en) * 2014-04-04 2015-10-07 Paris Sciences et Lettres - Quartier Latin Transparent metal fluoride ceramic
CN105948751A (en) * 2016-04-21 2016-09-21 武汉理工大学 Neodymium-doped 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
EP3208253A1 (en) * 2016-02-16 2017-08-23 Centre National De La Recherche Scientifique Transparent fluoride ceramic material and a method for its preparation
CN107619280A (en) * 2017-10-12 2018-01-23 信阳师范学院 A kind of preparation method of stratiform calcirm-fluoride crystalline ceramics
CN107628813A (en) * 2017-09-25 2018-01-26 信阳师范学院 A kind of method for reducing fluorite mineral and preparing polycrystalline transparent ceramic sintering temperature
CN108640686A (en) * 2018-06-27 2018-10-12 武汉理工大学 A kind of europium yttrium is co-doped with calcirm-fluoride scintillating ceramic and preparation method thereof

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EP2927202A1 (en) * 2014-04-04 2015-10-07 Paris Sciences et Lettres - Quartier Latin Transparent metal fluoride ceramic
WO2015150584A1 (en) * 2014-04-04 2015-10-08 Paris Sciences Et Lettres - Quartier Latin Transparent metal fluoride ceramic
CN106536449A (en) * 2014-04-04 2017-03-22 巴黎科学与文学联大-拉丁区 Transparent metal fluoride ceramic
US9862648B2 (en) 2014-04-04 2018-01-09 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
WO2017140558A1 (en) 2016-02-16 2017-08-24 Centre National De La Recherche Scientifique Transparent fluoride ceramic material and a method for its preparation
CN105948751A (en) * 2016-04-21 2016-09-21 武汉理工大学 Neodymium-doped 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
CN107628813A (en) * 2017-09-25 2018-01-26 信阳师范学院 A kind of method for reducing fluorite mineral and preparing polycrystalline transparent ceramic sintering temperature
CN107619280A (en) * 2017-10-12 2018-01-23 信阳师范学院 A kind of preparation method of stratiform calcirm-fluoride crystalline ceramics
CN107619280B (en) * 2017-10-12 2021-01-15 信阳师范学院 Preparation method of layered calcium fluoride transparent ceramic
CN108640686A (en) * 2018-06-27 2018-10-12 武汉理工大学 A kind of europium yttrium is co-doped with calcirm-fluoride scintillating ceramic and preparation method thereof

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