CN102826850A - Barium fluoride up-conversion transparent ceramic and preparation method thereof - Google Patents
Barium fluoride up-conversion transparent ceramic and preparation method thereof Download PDFInfo
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- CN102826850A CN102826850A CN2012102968770A CN201210296877A CN102826850A CN 102826850 A CN102826850 A CN 102826850A CN 2012102968770 A CN2012102968770 A CN 2012102968770A CN 201210296877 A CN201210296877 A CN 201210296877A CN 102826850 A CN102826850 A CN 102826850A
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Abstract
The invention discloses a barium fluoride up-conversion transparent ceramic and a preparation method thereof, and belongs to the technical field of optically functional materials. The existing alumina up-conversion transparent ceramic has low up-conversion luminous efficiency and is prepared difficultly. The barium fluoride up-conversion transparent ceramic utilizes barium fluoride transparent ceramic as a matrix and comprises: by mole, 60 to 89% of barium fluoride, 10 to 25% of ytterbium fluoride, and 1 to 15% of one or more of fluorides of erbium, holmium, neodymium, thulium and promethium. The preparation method comprises the following steps of blending raw material nanometer powder according to the mole percentage, wherein barium fluoride powder has particle sizes of 20 to 80nm and rare earth fluoride powder has particle sizes of 10 to 90nm, pressing the blended raw material nanometer powder into a biscuit, pre-sintering the biscuit at a temperature of 500 to 800 DEG C for 0.5 to 5 hours, carrying out vacuum sintering of the pre-sintered biscuit under the conditions of pressure of 50 to 500MPa, a vacuum degree of 10<-2> to 10<-3>Pa, a heating rate of 1 to 20 DEG C/min, a sintering temperature of 600 to 1200 DEG C and sintering time of 0.5 to 5 hours, and cooling to a room temperature at a rate of 1 to 20 DEG C/min to obtain the barium fluoride up-conversion transparent ceramic.
Description
Technical field
The present invention relates to conversion crystalline ceramics and preparation method thereof on a kind of barium fluoride, obtain the barium fluoride crystalline ceramics of conversion performance on having through mixing, belong to the optical function material technical field at barium fluoride matrix middle-weight rare earths.
Background technology
Last conversion crystalline ceramics is as a kind of novel transparent up-conversion; Both had last conversion performance; Good properties of transparency is arranged again; The characteristics of optical property and crystalline ceramics are combined, and are a kind of optical function materials of excellent property, can be used in the making of infrared detector, Laser Devices etc.
The existing conversion crystalline ceramics of going up belongs to oxide compound series, changes crystalline ceramics like going up of rear-earth-doped oxidation aluminum matrix.Its method of manufacture is to adopt liquid phase method to prepare presoma earlier; Presoma is through obtaining the sosoloid of aluminum oxide and rare earth oxide after calcining; Just prepare the needed material powder of conversion crystalline ceramics on the aluminum oxide, this powder obtains changing on the aluminum oxide crystalline ceramics through vacuum sintering.Yet; The doping concentration of rare earth ion of conversion crystalline ceramics is lower on the existing aluminum oxide, and therefore, its up-conversion luminescence efficiency ratio is lower; Last conversion performance is relatively poor, these drawbacks limit its make Application for Field as a kind of optical function material at infrared detector, Laser Devices etc.In addition, aspect the preparation method of conversion crystalline ceramics, liquid phase method prepares the technology more complicated of presoma on existing aluminum oxide; The factor that influences the material powder quality is also a lot, and material powder purity, the tiny uniformity coefficient of particle diameter, dispersiveness are difficult to guarantee; Sintering temperature is high, sintering time is long, vacuum tightness is high, as reaching 10
-4More than the Pa.
Summary of the invention
Its purpose of the present invention is, a kind of upward conversion crystalline ceramics that is easy to prepare and have higher up-conversion luminescence efficient is provided, and we have invented conversion crystalline ceramics and preparation method thereof on a kind of barium fluoride for this reason.
Conversion crystalline ceramics doping with rare-earth ions in crystalline ceramics matrix on the present invention's the barium fluoride; It is characterized in that; Said crystalline ceramics matrix is the barium fluoride crystalline ceramics; Its molar percentage proportioning of conversion crystalline ceramics is on the said barium fluoride: barium fluoride 60 ~ 89 %, fluoridize ytterbium 10 ~ 25%, one or more 1 ~ 15 % of the fluorochemical of erbium, holmium, neodymium, thulium, promethium.
Conversion crystalline ceramics preparation method comprises the vacuum sintering of crystalline ceramics on the present invention's the barium fluoride; It is characterized in that; According to final product molar percentage proportioning---barium fluoride 60 ~ 89 %, fluoridize ytterbium 10 ~ 25%; And one or more 1 ~ 15 % preparation of nano material powders of fluorochemical of erbium, holmium, neodymium, thulium, promethium, and its particle diameter of barium fluoride powder is in 20 ~ 80 nm scopes; Said various its particle diameter of rare earth fluorine powder is in 10 ~ 90 nm scopes; The preparation of nano material powder is pressed into biscuit, then pre-burning biscuit 0.5 ~ 5 hour under 500 ~ 800 ℃ of temperature; Biscuit after the vacuum sintering pre-burning applies the pressure of 50 ~ 500 MPa on biscuit, vacuum tightness is 10
-2~ 10
-3Pa, 1 ~ 20 ℃/min of temperature rise rate, sintering temperature is 600 ~ 1200 ℃, sintering time 0.5 ~ 5 hour, the speed with 1 ~ 20 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride.
Its technique effect of the present invention is that the substrate material barium fluoride of conversion crystalline ceramics has the low characteristics of phonon energy on the final product barium fluoride, and; Barium fluoride crystalline ceramics doping concentration of rare earth ion is high; Therefore, the up-conversion luminescence efficient of conversion crystalline ceramics is high on the barium fluoride, Given this; With respect to changing crystalline ceramics on the existing aluminum oxide, the conversion crystalline ceramics has better upward conversion performance on the present invention's the barium fluoride.Up-conversion luminescence intensity reflects up-conversion luminescence efficient can find out that from the detected result to the present invention's final product luminous intensity the present invention's final product has higher up-conversion luminescence efficient, sees shown in the accompanying drawing.And ceramic dense degree >=90 % of conversion crystalline ceramics on the barium fluoride reach more than 80 % in transmitance visible, near-infrared band.In addition, aspect the preparation method, the present invention does not prepare presoma, and technology is greatly simplified; Adopt the nano raw material powder, sintering temperature is very low, sintering time is extremely short, and vacuum tightness reduces an one magnitude, and these measures make the present invention's method processing condition become loose.
Description of drawings
Accompanying drawing is a conversion crystalline ceramics luminous intensity and emission wavelength graph of relation on the present invention's the final product barium fluoride, and this figure while is as Figure of abstract.
Embodiment
The specific embodiment of the invention is following.
Conversion crystalline ceramics doping with rare-earth ions in crystalline ceramics matrix on the present invention's the barium fluoride; Said crystalline ceramics matrix is the barium fluoride crystalline ceramics; Its molar percentage proportioning of conversion crystalline ceramics is on the said barium fluoride: barium fluoride 60 ~ 89 %; Fluoridize ytterbium 10 ~ 25%, one or more 1 ~ 15 % of the fluorochemical of erbium, holmium, neodymium, thulium, promethium.
Conversion crystalline ceramics preparation method comprises the vacuum sintering of crystalline ceramics on the present invention's the barium fluoride, specifically may further comprise the steps:
1, preparation of nano material powder
According to final product molar percentage proportioning---barium fluoride 60 ~ 89 %, fluoridize ytterbium 10 ~ 25%; And one or more 1 ~ 15 % preparation of nano material powders of fluorochemical of erbium, holmium, neodymium, thulium, promethium; And its particle diameter of barium fluoride powder is in 20 ~ 80 nm scopes; Said various its particle diameter of rare earth fluorine powder is in 10 ~ 90 nm scopes.
Wherein the preparation process of barium fluoride powder does, with chemically pure reagent Ba (NO
3)
2Be dissolved in the deionized water, be mixed with the solution that volumetric molar concentration is 0.05 ~ 0.33M, add excessive Neutral ammonium fluoride then, generate barium fluoride (BaF
2) deposition, stir with the stir speed (S.S.) of 200 ~ 500rpm and to obtain barium fluoride suspension-s, through the drying of 12 ~ 48 hours ageings, water or alcohol wash and 12 ~ 48 hours, obtain pure phase cube barium fluoride powder again.
Wherein the preparation process of rare earth fluorine powder does, with chemically pure reagent Re
2O
3(rare earth oxide) adds in the nitric acid and heating for dissolving; Be mixed with the solution that concentration is 0.05 ~ 5M; Add Neutral ammonium fluoride then, generate the rare earth fluorine deposition, stir with the stir speed (S.S.) of 200 ~ 500rpm and obtain rare earth fluorine suspension-s; Through the drying of 12 ~ 48 hours ageings, water or alcohol wash and 12 ~ 48 hours, obtain the rare earth fluorine powder again.
Barium fluoride powder, rare earth fluorine powder are adopted dry grinding method or wet milling process ball milling 12 ~ 48 hours, obtain the nano raw material powder.
2, make biscuit
With dry-pressing formed mode the preparation of nano material powder is pressed into biscuit, axle pressure is 5 ~ 30MPa, under 200 ~ 300MPa pressure, carries out isostatic cool pressing again and handles; Then in retort furnace under 500 ~ 800 ℃ of temperature pre-burning biscuit 0.5 ~ 5 hour.
3, vacuum sintering
Biscuit in the vacuum heating-press sintering stove after the vacuum sintering pre-burning applies the pressure of 50 ~ 500 MPa on biscuit, vacuum tightness is 10
-2~ 10
-3Pa, 1 ~ 20 ℃/min of temperature rise rate, sintering temperature is 600 ~ 1200 ℃, sintering time 0.5 ~ 5 hour, the speed with 1 ~ 20 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride.
Further specify the present invention below for example.
Embodiment 1: according to technical process, with chemically pure reagent Ba (NO
3)
2Be dissolved in the deionized water, be mixed with the solution that volumetric molar concentration is 0.2M, add excessive Neutral ammonium fluoride then, generate barium fluoride (BaF
2) deposition, stir with the stir speed (S.S.) of 200rpm and to obtain barium fluoride suspension-s, clean through ageing in 14 hours, water again and 14 hours drying, obtain pure phase cube barium fluoride powder, its median size is 40nm.With chemically pure reagent Yb
2O
3(ytterbium oxide) adds in the nitric acid and heating for dissolving, is mixed with the solution that concentration is 2M, adds Neutral ammonium fluoride then, generates YbF
3(fluoridizing ytterbium) deposition stirs with the stir speed (S.S.) of 300rpm and to obtain YbF
3Suspension-s cleans through ageing in 24 hours, water and 24 hours drying again, obtains fluoridizing the ytterbium powder, and its median size is 50nm.Same preparation median size with fluoridize the ytterbium powder identical fluoridize erbium (ErF
3) powder.According to molar percentage BaF
270%, YbF
320%, ErF
3Each nano raw material powder of 10% weighing adopted dry grinding method ball milling raw material 12 hours, obtained blended nano raw material powder.The mixing nano raw material powder that to prepare with dry-pressing formed mode is pressed into biscuit, and axle pressure is 10MPa, under 200MPa pressure, carries out isostatic cool pressing again and handles; Then in retort furnace under 600 ℃ of temperature pre-burning biscuit 2 hours.Biscuit in the vacuum heating-press sintering stove after the vacuum sintering pre-burning applies the pressure of 100 MPa on biscuit, vacuum tightness is 10
-3Pa, 4 ℃/min of temperature rise rate, sintering temperature is 900 ℃; Sintering time 1 hour, the speed with 5 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride; Its density>=90 % reaches more than 80 % in transmitance visible, near-infrared band, adopts the irradiation of 980nm infrared light; The up-conversion luminescence wavelength is 550nm, and eye-observation is a bright green, sees shown in the accompanying drawing.
Embodiment 2: according to technical process, with chemically pure reagent Ba (NO
3)
2Be dissolved in the deionized water, be mixed with the solution that volumetric molar concentration is 0.2M, add excessive Neutral ammonium fluoride then, generate barium fluoride (BaF
2) deposition, stir with the stir speed (S.S.) of 200rpm and to obtain barium fluoride suspension-s, clean through ageing in 14 hours, water again and 14 hours drying, obtain pure phase cube barium fluoride powder, its median size is 40nm.With chemically pure reagent Yb
2O
3(ytterbium oxide) adds in the nitric acid and heating for dissolving, is mixed with the solution that concentration is 2M, adds Neutral ammonium fluoride then, generates YbF
3(fluoridizing ytterbium) deposition stirs with the stir speed (S.S.) of 300rpm and to obtain YbF
3Suspension-s cleans through ageing in 24 hours, water and 24 hours drying again, obtains fluoridizing the ytterbium powder, and its median size is 50nm.Same preparation median size with fluoridize the ytterbium powder identical fluoridize erbium (ErF
3) powder, holmium fluoride (HoF
3) powder and neodymium fluoride (NdF
3) powder.According to molar percentage BaF
265%, YbF
325%, ErF
3+ HoF
3+ NdF
3Each nano raw material powder of totally 10% weighing adopted dry grinding method ball milling raw material 24 hours, obtained blended nano raw material powder.The mixing nano raw material powder that to prepare with dry-pressing formed mode is pressed into biscuit, and axle pressure is 15MPa, under 240MPa pressure, carries out isostatic cool pressing again and handles; Then in retort furnace under 650 ℃ of temperature pre-burning biscuit 2 hours.Biscuit in the vacuum heating-press sintering stove after the vacuum sintering pre-burning applies the pressure of 100 MPa on biscuit, vacuum tightness is 10
-3Pa, 5 ℃/min of temperature rise rate, sintering temperature is 900 ℃, sintering time 1 hour, the speed with 5 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride.
Embodiment 3: according to technical process, with chemically pure reagent Ba (NO
3)
2Be dissolved in the deionized water, be mixed with the solution that volumetric molar concentration is 0.2M, add excessive Neutral ammonium fluoride then, generate barium fluoride (BaF
2) deposition, stir with the stir speed (S.S.) of 200rpm and to obtain barium fluoride suspension-s, clean through ageing in 14 hours, water again and 14 hours drying, obtain pure phase cube barium fluoride powder, its median size is 40nm.With chemically pure reagent Yb
2O
3(ytterbium oxide) adds in the nitric acid and heating for dissolving, is mixed with the solution that concentration is 2M, adds Neutral ammonium fluoride then, generates YbF
3(fluoridizing ytterbium) deposition stirs with the stir speed (S.S.) of 300rpm and to obtain YbF
3Suspension-s cleans through ageing in 24 hours, water and 24 hours drying again, obtains fluoridizing the ytterbium powder, and its median size is 50nm.Same preparation median size with fluoridize the ytterbium powder identical fluoridize erbium (ErF
3) powder.According to molar percentage BaF
280%, YbF
316%, ErF
3Each nano raw material powder of 4% weighing adopted dry grinding method ball milling raw material 24 hours, obtained blended nano raw material powder.The mixing nano raw material powder that to prepare with dry-pressing formed mode is pressed into biscuit, and axle pressure is 15MPa, under 260MPa pressure, carries out isostatic cool pressing again and handles; Then in retort furnace under 700 ℃ of temperature pre-burning biscuit 1 hour.Biscuit in the vacuum heating-press sintering stove after the vacuum sintering pre-burning applies the pressure of 100 MPa on biscuit, vacuum tightness is 10
-3Pa, 3 ℃/min of temperature rise rate, sintering temperature is 1000 ℃, sintering time 1 hour, the speed with 3 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride.
Embodiment 4: according to technical process, with chemically pure reagent Ba (NO
3)
2Be dissolved in the deionized water, be mixed with the solution that volumetric molar concentration is 0.2M, add excessive Neutral ammonium fluoride then, generate barium fluoride (BaF
2) deposition, stir with the stir speed (S.S.) of 200rpm and to obtain barium fluoride suspension-s, clean through ageing in 14 hours, water again and 14 hours drying, obtain pure phase cube barium fluoride powder, its median size is 40nm.With chemically pure reagent Yb
2O
3(ytterbium oxide) adds in the nitric acid and heating for dissolving, is mixed with the solution that concentration is 2M, adds Neutral ammonium fluoride then, generates YbF
3(fluoridizing ytterbium) deposition stirs with the stir speed (S.S.) of 300rpm and to obtain YbF
3Suspension-s cleans through ageing in 24 hours, water and 24 hours drying again, obtains fluoridizing the ytterbium powder, and its median size is 50nm.Same preparation median size with fluoridize the ytterbium powder identical fluoridize erbium (ErF
3) powder with fluoridize thulium (TmF
3) powder.According to molar percentage BaF
275%, YbF
320%, ErF
3+ TmF
3Each nano raw material powder of totally 5% weighing adopted dry grinding method ball milling raw material 24 hours, obtained blended nano raw material powder.The mixing nano raw material powder that to prepare with dry-pressing formed mode is pressed into biscuit, and axle pressure is 20MPa, under 200MPa pressure, carries out isostatic cool pressing again and handles; Then in retort furnace under 700 ℃ of temperature pre-burning biscuit 1 hour.Biscuit in the vacuum heating-press sintering stove after the vacuum sintering pre-burning applies the pressure of 100 MPa on biscuit, vacuum tightness is 10
-3Pa, 3 ℃/min of temperature rise rate, sintering temperature is 1000 ℃, sintering time 1 hour, the speed with 3 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride.
Embodiment 5: according to technical process, with chemically pure reagent Ba (NO
3)
2Be dissolved in the deionized water, be mixed with the solution that volumetric molar concentration is 0.2M, add excessive Neutral ammonium fluoride then, generate barium fluoride (BaF
2) deposition, stir with the stir speed (S.S.) of 200rpm and to obtain barium fluoride suspension-s, clean through ageing in 14 hours, water again and 14 hours drying, obtain pure phase cube barium fluoride powder, its median size is 40nm.With chemically pure reagent Yb
2O
3(ytterbium oxide) adds in the nitric acid and heating for dissolving, is mixed with the solution that concentration is 2M, adds Neutral ammonium fluoride then, generates YbF
3(fluoridizing ytterbium) deposition stirs with the stir speed (S.S.) of 300rpm and to obtain YbF
3Suspension-s cleans through ageing in 24 hours, water and 24 hours drying again, obtains fluoridizing the ytterbium powder, and its median size is 50nm.Same preparation median size with fluoridize the ytterbium powder identical fluoridize erbium (ErF
3) powder with fluoridize promethium (PmF
3) powder.According to molar percentage BaF
278%, YbF
316%, ErF
3+ PmF
3Each nano raw material powder of totally 6% weighing adopted dry grinding method ball milling raw material 36 hours, obtained blended nano raw material powder.The mixing nano raw material powder that to prepare with dry-pressing formed mode is pressed into biscuit, and axle pressure is 20MPa, under 250MPa pressure, carries out isostatic cool pressing again and handles; Then in retort furnace under 750 ℃ of temperature pre-burning biscuit 2 hours.Biscuit in the vacuum heating-press sintering stove after the vacuum sintering pre-burning applies the pressure of 100 MPa on biscuit, vacuum tightness is 10
-3Pa, 3 ℃/min of temperature rise rate, sintering temperature is 1000 ℃, sintering time 1 hour, the speed with 3 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride.
Embodiment 6: according to technical process, with chemically pure reagent Ba (NO
3)
2Be dissolved in the deionized water, be mixed with the solution that volumetric molar concentration is 0.2M, add excessive Neutral ammonium fluoride then, generate barium fluoride (BaF
2) deposition, stir with the stir speed (S.S.) of 200rpm and to obtain barium fluoride suspension-s, clean through ageing in 14 hours, water again and 14 hours drying, obtain pure phase cube barium fluoride powder, its median size is 40nm.With chemically pure reagent Yb
2O
3(ytterbium oxide) adds in the nitric acid and heating for dissolving, is mixed with the solution that concentration is 2M, adds Neutral ammonium fluoride then, generates YbF
3(fluoridizing ytterbium) deposition stirs with the stir speed (S.S.) of 300rpm and to obtain YbF
3Suspension-s cleans through ageing in 24 hours, water and 24 hours drying again, obtains fluoridizing the ytterbium powder, and its median size is 50nm.Same preparation median size with fluoridize the ytterbium powder identical fluoridize erbium (ErF
3) powder.According to molar percentage BaF
280%, YbF
316%, ErF
3Each nano raw material powder of 4% weighing adopted dry grinding method ball milling raw material 48 hours, obtained blended nano raw material powder.The mixing nano raw material powder that to prepare with dry-pressing formed mode is pressed into biscuit, and axle pressure is 30MPa, under 300MPa pressure, carries out isostatic cool pressing again and handles; Then in retort furnace under 800 ℃ of temperature pre-burning biscuit 3 hours.Biscuit in the vacuum heating-press sintering stove after the vacuum sintering pre-burning applies the pressure of 100 MPa on biscuit, vacuum tightness is 10
-3Pa, 10 ℃/min of temperature rise rate, sintering temperature is 1200 ℃, sintering time 5 hours, the speed with 10 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride.
Embodiment 7: according to technical process, with chemically pure reagent Ba (NO
3)
2Be dissolved in the deionized water, be mixed with the solution that volumetric molar concentration is 0.2M, add excessive Neutral ammonium fluoride then, generate barium fluoride (BaF
2) deposition, stir with the stir speed (S.S.) of 200rpm and to obtain barium fluoride suspension-s, clean through ageing in 14 hours, water again and 14 hours drying, obtain pure phase cube barium fluoride powder, its median size is 40nm.With chemically pure reagent Yb
2O
3(ytterbium oxide) adds in the nitric acid and heating for dissolving, is mixed with the solution that concentration is 2M, adds Neutral ammonium fluoride then, generates YbF
3(fluoridizing ytterbium) deposition stirs with the stir speed (S.S.) of 300rpm and to obtain YbF
3Suspension-s cleans through ageing in 24 hours, water and 24 hours drying again, obtains fluoridizing the ytterbium powder, and its median size is 50nm.Same preparation median size with fluoridize the ytterbium powder identical fluoridize erbium (ErF
3) powder.According to molar percentage BaF
280%, YbF
318%, ErF
3Each nano raw material powder of 2% weighing adopted dry grinding method ball milling raw material 12 hours, obtained blended nano raw material powder.The mixing nano raw material powder that to prepare with dry-pressing formed mode is pressed into biscuit, and axle pressure is 5MPa, under 200MPa pressure, carries out isostatic cool pressing again and handles; Then in retort furnace under 500 ℃ of temperature pre-burning biscuit 1 hour.Biscuit in the vacuum heating-press sintering stove after the vacuum sintering pre-burning applies the pressure of 100 MPa on biscuit, vacuum tightness is 10
-3Pa, 3 ℃/min of temperature rise rate, sintering temperature is 800 ℃, sintering time 0.5 hour, the speed with 3 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride.
Claims (6)
1. change crystalline ceramics on a barium fluoride; Doping with rare-earth ions in crystalline ceramics matrix; It is characterized in that said crystalline ceramics matrix is the barium fluoride crystalline ceramics, its molar percentage proportioning of conversion crystalline ceramics is on the said barium fluoride: barium fluoride 60 ~ 89 %; Fluoridize ytterbium 10 ~ 25%, one or more 1 ~ 15 % of the fluorochemical of erbium, holmium, neodymium, thulium, promethium.
2. change the crystalline ceramics preparation method on a barium fluoride; Comprise the vacuum sintering of crystalline ceramics; It is characterized in that, according to final product molar percentage proportioning---barium fluoride 60 ~ 89 %, fluoridize ytterbium 10 ~ 25%, and one or more 1 ~ 15 % preparation of nano material powders of fluorochemical of erbium, holmium, neodymium, thulium, promethium; And its particle diameter of barium fluoride powder is in 20 ~ 80 nm scopes; Said various its particle diameter of rare earth fluorine powder is in 10 ~ 90 nm scopes; The preparation of nano material powder is pressed into biscuit, then pre-burning biscuit 0.5 ~ 5 hour under 500 ~ 800 ℃ of temperature; Biscuit after the vacuum sintering pre-burning applies the pressure of 50 ~ 500 MPa on biscuit, vacuum tightness is 10
-2~ 10
-3Pa, 1 ~ 20 ℃/min of temperature rise rate, sintering temperature is 600 ~ 1200 ℃, sintering time 0.5 ~ 5 hour, the speed with 1 ~ 20 ℃/min is cooled to room temperature at last, obtains changing crystalline ceramics on the final product barium fluoride.
3. conversion crystalline ceramics preparation method is characterized in that wherein the preparation process of barium fluoride powder does, with chemically pure reagent Ba (NO on the barium fluoride according to claim 2
3)
2Be dissolved in the deionized water, be mixed with the solution that volumetric molar concentration is 0.05 ~ 0.33M, add excessive Neutral ammonium fluoride then, generate barium fluoride (BaF
2) deposition, stir with the stir speed (S.S.) of 200 ~ 500rpm and to obtain barium fluoride suspension-s, through the drying of 12 ~ 48 hours ageings, water or alcohol wash and 12 ~ 48 hours, obtain pure phase cube barium fluoride powder again.
4. conversion crystalline ceramics preparation method is characterized in that wherein the preparation process of rare earth fluorine powder does, with chemically pure reagent Re on the barium fluoride according to claim 2
2O
3Add in the nitric acid and heating for dissolving; Be mixed with the solution that concentration is 0.05 ~ 5M; Add Neutral ammonium fluoride then, generate the rare earth fluorine deposition, stir with the stir speed (S.S.) of 200 ~ 500rpm and obtain rare earth fluorine suspension-s; Through the drying of 12 ~ 48 hours ageings, water or alcohol wash and 12 ~ 48 hours, obtain the rare earth fluorine powder again.
5. conversion crystalline ceramics preparation method is characterized in that on the barium fluoride according to claim 2, and barium fluoride powder, rare earth fluorine powder were adopted dry grinding method or wet milling process ball milling 12 ~ 48 hours, obtains the nano raw material powder.
6. conversion crystalline ceramics preparation method on the barium fluoride according to claim 2; It is characterized in that; With dry-pressing formed mode the preparation of nano material powder is pressed into biscuit, axle pressure is 5 ~ 30MPa, under 200 ~ 300MPa pressure, carries out isostatic cool pressing again and handles; Pre-burning biscuit in retort furnace then.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103275706A (en) * | 2013-05-31 | 2013-09-04 | 湘潭大学 | Blue up-conversion luminescent material and preparation method thereof |
| CN104177092A (en) * | 2013-05-20 | 2014-12-03 | 中国科学院上海硅酸盐研究所 | Method for preparing transparent luminescent ceramic |
| CN105271777A (en) * | 2015-11-27 | 2016-01-27 | 宁波大学 | Rare-earth ion doped Rb2LaBr5 microcrystalline glass 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 |
| CN113548894A (en) * | 2021-07-15 | 2021-10-26 | 中国科学院上海硅酸盐研究所 | Ytterbium-yttria up-conversion luminescent transparent ceramic and preparation method thereof |
-
2012
- 2012-08-20 CN CN2012102968770A patent/CN102826850A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 刘全生等: "Ho3+/Tm3+掺杂氟磷酸盐玻璃的研究", 《武汉理工大学学报》 * |
| 袁放成等: "氟化物玻璃陶瓷中Er的上转换特性", 《湘潭大学自然科学学报》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177092A (en) * | 2013-05-20 | 2014-12-03 | 中国科学院上海硅酸盐研究所 | Method for preparing transparent luminescent ceramic |
| CN103275706A (en) * | 2013-05-31 | 2013-09-04 | 湘潭大学 | Blue up-conversion luminescent material and preparation method thereof |
| CN105271777A (en) * | 2015-11-27 | 2016-01-27 | 宁波大学 | Rare-earth ion doped Rb2LaBr5 microcrystalline glass 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 |
| CN113548894A (en) * | 2021-07-15 | 2021-10-26 | 中国科学院上海硅酸盐研究所 | Ytterbium-yttria up-conversion luminescent transparent ceramic and preparation method thereof |
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