CN104264223A - Growth method for alpha-NaYF4 (cubic sodium yttrium fluoride) monocrystals - Google Patents
Growth method for alpha-NaYF4 (cubic sodium yttrium fluoride) monocrystals Download PDFInfo
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- CN104264223A CN104264223A CN201410556977.1A CN201410556977A CN104264223A CN 104264223 A CN104264223 A CN 104264223A CN 201410556977 A CN201410556977 A CN 201410556977A CN 104264223 A CN104264223 A CN 104264223A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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Abstract
The invention discloses a growth method for alpha-NaYF4 (cubic sodium yttrium fluoride) monocrystals. The growth method is characterized in that the alpha-NaYF4 monocrystals are obtained through Steps (1)-(4); KF (potassium fluoride) is added in Step (1) as a cosolvent; in Step (2), raw materials are treated with HF (hydrogen fluoride) treatment for 1 to 5 hours at a high temperature ranging from 780 DEG C to 800 DEG C; a Pt (platinum) crucible is sealed in Step (3); in Step (4), the crystal growth is carried out through the Bridgman-Stockbarger Method with the cosolvent, that is, the sealed Pt crucible is placed in a molybdenum disilicide rod electric furnace to carry out the crystal growth through the Bridgman-Stockbarger Method; the crystal growth parameters are as follows: the furnace body temperature ranges from 950 DEG C to 980 DEG C, the inoculation temperature ranges from 820 DEG C to 860 DEG C, the temperature gradient of the solid-liquid interphase ranges from 50 DEG C per centimeter to 90 DEG C per centimeter, and the crucible descending speed ranges from 0.2 millimeter per hour to 2.0 millimeters per hour; after the crystal growth is completed, the furnace temperature is reduced to the room temperature at a rate of 20 to 80 DEG C per hour, so that the alpha-NaYF4 monocrystals with a larger size and a higher quality can be obtained. The growth method has the advantage that the transmittances of the crystals within the waveband of 200 to 8,700 nanometers all exceed 80 percent, so that the alpha-NaYF4 crystals achieve wider application prospects for mid-infrared optical devices.
Description
Technical field
The present invention relates to crystal growth, be specifically related to a kind of Emission in Cubic yttrium fluoride natrium (α-NaYF
4) growth method of single crystal.
Background technology
NaYF
4features such as being a kind of excellent optical substrate material found nearly decades, it has, and phonon energy is low, doping with rare-earth ions luminous efficiency is high, transmitance that is visible and infrared band is high, physical and chemical performance is stable.At NaYF
4rare earth ion is mixed in matrix, can NaYF
4superior optical characteristics combine with the specificity of active rare-earth ion, obtain and there is the type material of many excellent specific properties.Under normal conditions, it has Emission in Cubic (α-NaYF
4) with six side's phase (β-NaYF
4) two kinds of crystalline structure.Such as, with six side phase β-NaYF
4for matrix, the β-NaYF of Yb and Er codoped
4one of the highest up-conversion luminescent material of efficiency of conversion gone up up to now by material.Therefore NaYF
4be with a wide range of applications in high-sensitive biomolecules fluorescence, three stereo display, infrared acquisition, solid statelaser, the field such as false proof.
Up to the present, relevant NaYF
4the report of material all concentrates on micro-crystalline material, if publication number is the patent of invention of CN102660287A, then disclose a kind of six sides mutually on change NaYF
4the preparation method of nano material, but can produce strong scattering to light due to nano microcrystalline powdered material, therefore badly influences the transmitance of device, thus limits it and apply widely.Therefore high-quality, transparent large size NaYF is synthesized
4single crystal has great using value.
From NaF-YF
3phase equilibrium diagram (Inorganic Chemistry, 1963,2 (5): 1005 ~ 1012) in can draw, all containing α-NaYF
4crystal region, separate out α-NaYF from melt
4also separate out other Solid solution material while single crystal, because multiple solid matter is separated out in the melt simultaneously, be therefore difficult to the α-NaYF obtaining large-size
4single crystal; For β-NaYF
4crystallization phases region, only as NaF and YF
3original components proportioning greatly about (72-68mol%): time (28-32mol%), just likely crystallization obtains β-NaYF in theory
4single crystal, therefore from original ingredient only have at most ~ 25mol% can crystallization go out β-NaYF
4crystal, the impurity residued in melt has a strong impact on growing up and the quality of crystal of crystal.Therefore up to the present α-NaYF is not also had at home and abroad
4with β-NaYF
4effective growth method report of large size single crystal body.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of α-NaYF that can grow large-size
4the growth method of single crystal.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of α-NaYF
4the growth method of single crystal, comprises the steps:
1, the preparation of growth raw material and high-temperature fluorination process:
Purity is greater than NaF, KF and the YF of 99.99%
31 ~ 2.40: 1: 2.24 ~ 3.40 mixing in molar ratio, be placed in device for grinding, mill mixing 5 ~ 6h, obtains uniform powder;
Above-mentioned compound is placed in Platinum crucible, and Platinum crucible is installed in the platinum pipeline of tube type resistance furnace, then uses N
2gas gets rid of the ducted air of platinum, and temperature 780 ~ 800 DEG C, under logical HF gas, reaction treatment 1 ~ 5 hour, reaction treatment terminates, and closes HF gas and tube type resistance furnace, uses N
2hF gas residual in gas pipe blow-through, all remaining HF gas through pipeline tail end is reclaimed by NaOH solution, finally obtains polycrystalline powder;
2, crystal growth:
Using KF as fusing assistant, sealing crucible descent method is adopted to carry out crystal growth, above-mentioned polycrystalline powder is placed in device for grinding clay into power, then Pt crucible is placed in and compacting, sealing Pt crucible, sealing has just completely cut off air and steam, makes to completely cut off with air and steam in crystal growing process, makes the α-NaYF of growth
4single crystal quality is high;
The Pt crucible of sealing is placed in Si-Mo rod stove, use Bridgman-Stockbarge method for growing crystal, the parameter of growing crystal is: furnace body temperature is 950 ~ 980 DEG C, inoculation temp is 820 ~ 860 DEG C, the thermograde of solid-liquid interface is 50 ~ 90 DEG C/cm, and crucible lowering speed is 0.2 ~ 2.0mm/h, adopts larger thermograde, be convenient to the growth controlling crystal, comparatively large and that quality is higher α-NaYF can be obtained
4single crystal;
3, crystal annealing:
Adopt the method for in-situ annealing, after crystal growth terminates, with 20 ~ 80 DEG C/h decline furnace temperature to room temperature, obtain α-NaYF
4single crystal.
Compared with prior art, the invention has the advantages that: (1) is at α-NaYF
4during crystal growing process, in initial feed, adding a certain amount of KF (fusing point 858 DEG C), as fusing assistant, fusing assistant KF reduces α-NaYF
4the fusing point of crystal, changes the phase equilibrium relationship in melt, thus makes when melt starts initial stage crystallization, only single precipitation α-NaYF
4solid-state phase and other liquid phase, along with α-NaYF
4the nucleation and growth of crystal, the final α-NaYF obtaining large-size
4crystal; (2) α-NaYF
4crystal has the through performance of wide range, and the transmitance of 200 ~ 8700nm wave band is all more than 80%, and similar LiYF of the same clan
4single crystal only in the transmitance of 200 ~ 6370nm wave band more than 80%, therefore α-NaYF
4crystal will have larger application prospect in mid-infrared light device; (3) use of fusing assistant KF, makes crystal growth temperature decline, thus effectively reduces because the volatilization of fluorochemical may to the injury of the loss of equipment and human body in process of growth, again can brownout cost; (4) α-NaYF for preparing of the present invention's crucible descent method
4single crystal, due to multi-tube furnace can be adopted to produce, namely a production cycle can obtain many crystal simultaneously, therefore can increase substantially output and the preparation cost reducing material, this preparation method's technique is simple, and single crystal purity is high, quality better, is convenient to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the α-NaYF of embodiment 1
4single crystal samples figure;
Fig. 2 is the α-NaYF that embodiment 1 obtains
4monocrystalline and standard α-NaYF
4x-ray powder diffraction (XRD) comparison diagram;
Fig. 3 is the α-NaYF of embodiment 1
4monocrystalline and LiYF
4monocrystalline through spectrum comparison diagram.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1:
According to NaF:KF: YF
3mol ratio be 1.25: 1.00: 2.48, take respectively purity be all greater than the NaF raw material of 99.99%, the KF raw material of 99.99% and 99.99% YF
3raw material, mixing is placed in device for grinding, and mixing 5.5 hours of milling, obtains the compound of uniform powder; Be put in fluffy for compound in boat-shaped Platinum crucible, then this boat-shaped Platinum crucible is installed in the platinum pipeline of tube type resistance furnace, then use high-purity N
2the ducted air of this platinum of air scavenge, and this platinum pipeline is hunted leak; Afterwards the furnace body temperature of tube type resistance furnace is elevated to 790 DEG C gradually, logical HF gas, reacts 2 hours, removes the H that may contain
2o and oxyfluoride, absorb the HF gas in tail gas by NaOH solution in reaction process, after reaction terminates, stops logical HF gas, close tube type resistance furnace, finally use high-purity N
2hF gas residual in air scavenge platinum pipeline, obtains rare earth ion doped polycrystalline powder; Polycrystalline powder is placed in device for grinding and is milled into powder, then this powder is placed in platinum crucible and compacting, then seal this platinum crucible; The platinum crucible of sealing is placed in Si-Mo rod stove, use Bridgman-Stockbarge method for growing crystal, the parameter of growing crystal is: furnace body temperature is 960 DEG C, inoculation temp is 830 DEG C, the thermograde of solid-liquid interface is 70 DEG C/cm, driving device lowering means decline crucible carries out crystal growth, and crucible lowering speed is 1.0mm/h; After crystal growth terminates, with 50 DEG C/h decline furnace temperature to room temperature.Peel platinum crucible off and obtain blank crystal.Fig. 1 is the crystal prototype figure that embodiment 1 obtains, and bottom is transparent clear crystal, and top is the opaque precipitate of white.Fig. 2 is transparent single crystal body X-ray powder diffraction figure (XRD) of embodiment 1, with the α-NaYF of standard
4the XRD (card number: JCPD77-2042) of crystal is consistent, and the single crystal therefore obtained is α-NaYF
4phase.
Reference examples 1:
According to LiF: YF
3mol ratio be 1.06: 1, take LiF raw material and YF that purity is all greater than 99.99%
3raw material, mixing is placed in device for grinding, and mixing 5.5 hours of milling, obtains the compound of uniform powder; Be put in fluffy for compound in boat-shaped Platinum crucible, then this boat-shaped Platinum crucible is installed in the platinum pipeline of tube type resistance furnace, then use high-purity N
2the ducted air of this platinum of air scavenge, and this platinum pipeline is hunted leak; Afterwards the furnace body temperature of tube type resistance furnace is elevated to 790 DEG C gradually, logical HF gas, reacts 2 hours, removes the H that may contain
2o and oxyfluoride, absorb the HF gas in tail gas by NaOH solution in reaction process, after reaction terminates, stops logical HF gas, close tube type resistance furnace, finally use high-purity N
2hF gas residual in air scavenge platinum pipeline, obtains rare earth ion doped polycrystalline powder; Polycrystalline powder is placed in device for grinding and is milled into powder, then this powder is placed in platinum crucible and compacting, then seal this platinum crucible; The platinum crucible of sealing is placed in Si-Mo rod stove, use Bridgman-Stockbarge method for growing crystal, the parameter of growing crystal is: furnace body temperature is ~ 950 DEG C, inoculation temp is 830 DEG C, the thermograde of solid-liquid interface is 70 DEG C/cm, driving device lowering means decline crucible carries out crystal growth, and crucible speed is 1.0mm/h; After crystal growth terminates, with 50 DEG C/h decline furnace temperature to room temperature, obtain LiYF
4single crystal.
α-the NaYF that embodiment 1 is obtained
4the LiYF that monocrystalline and reference examples 1 obtain
4single crystal respectively through cutting, and is polished to the thin slice that thickness is 2 millimeters, carries out the test through spectrum and contrast, the results are shown in Figure shown in 3.α-the NaYF that embodiment 1 obtains
4the transmitance from 200 ~ 8700nm wave band of single crystal is all more than 80%, and LiYF
4single crystal only in the transmitance of 200 ~ 6370nm wave band more than 80%, therefore α-NaYF
4single crystal compare LiYF through scope
4single crystal is wide, especially in middle-infrared band.
Embodiment 2
Substantially the same manner as Example 1, difference is raw material NaF: KF: YF
3mol ratio be 1: 1: 2.24, weighing also mixing is placed in device for grinding, to mill mixing 5 hours, be 5 hours with the HF gas reaction time in platinum pipeline, furnace body temperature 950 DEG C, inoculation temp is 820 DEG C, the thermograde of solid-liquid interface is 50 DEG C/cm, crystalline growth velocity is 0.2mm/h, and furnace temperature lowering speed is 80 DEG C/h, the XRD figure of crystal and substantially the same manner as Example 1 through spectrum.
Embodiment 3
Substantially the same manner as Example 1, difference is raw material NaF: KF: YF
3mol ratio be 2.40: 1: 3.40, weighing also mixing is placed in device for grinding, to mill mixing 6 hours, be 1 hour with the HF gas reaction time in platinum pipeline, furnace body temperature 980 DEG C, inoculation temp 860 DEG C, the thermograde of solid-liquid interface is 90 DEG C/cm, crystalline growth velocity is 2.0mm/h, and furnace temperature lowering speed is 20 DEG C/h, the XRD figure of crystal and substantially the same manner as Example 1 through spectrum.
Embodiment 4
Substantially the same manner as Example 1, difference is raw material NaF: KF: YF
3mol ratio be 1: 1: 3.40, weighing also mixing is placed in device for grinding, to mill mixing 5.5 hours, be 4 hours with the HF gas reaction time in platinum pipeline, furnace body temperature 960 DEG C, inoculation temp is 840 DEG C, the thermograde of solid-liquid interface is 75 DEG C/cm, crystalline growth velocity is 1.5mm/h, and furnace temperature lowering speed is 40 DEG C/h, the XRD figure of crystal and substantially the same manner as Example 1 through spectrum.
Embodiment 5
Substantially the same manner as Example 1, difference is raw material NaF: KF: YF
3mol ratio be 2.40: 1: 2.24, weighing also mixing is placed in device for grinding, to mill mixing 6 hours, be 3 hours with the HF gas reaction time in platinum pipeline, furnace body temperature 970 DEG C, inoculation temp 840 DEG C, the thermograde of solid-liquid interface is 55 DEG C/cm, crystalline growth velocity is 1.2mm/h, and furnace temperature lowering speed is 65 DEG C/h, the XRD figure of crystal and substantially the same manner as Example 1 through spectrum.
Embodiment 6
Substantially the same manner as Example 1, difference is raw material NaF: KF: YF
3mol ratio be 2.00: 1: 3.00, weighing also mixing is placed in device for grinding, to mill mixing 5.5 hours, be 3.5 hours with the HF gas reaction time in platinum pipeline, furnace body temperature 975 DEG C, inoculation temp 850 DEG C, the thermograde of solid-liquid interface is 85 DEG C/cm, crystalline growth velocity is 1.8mm/h, and furnace temperature lowering speed is 65 DEG C/h, the XRD figure of crystal and substantially the same manner as Example 1 through spectrum.
Claims (4)
1. a α-NaYF
4the growth method of single crystal, is characterized in that comprising the steps:
1), in molar ratio 1 ~ 2.40: 1: 2.24 ~ 3.40, NaF, KF, YF
3raw material is placed in device for grinding, and mill mixing 5 ~ 6h, obtains the compound of uniform powder;
2), by above-mentioned compound be placed in Platinum crucible, Platinum crucible is installed in the platinum pipeline of tube type resistance furnace, then uses N
2gas gets rid of the ducted air of platinum, and temperature 780 ~ 800 DEG C, under logical HF gas, reaction treatment 1 ~ 5 hour, reaction treatment terminates, and closes HF gas and tube type resistance furnace, uses N
2hF gas residual in gas pipe blow-through, all remaining HF gas through pipeline tail end is reclaimed by NaOH solution, finally obtains polycrystalline powder;
3), using KF as fusing assistant, adopt sealing crucible descent method to carry out crystal growth, above-mentioned polycrystalline powder is placed in device for grinding and clays into power, be then placed in Pt crucible and compacting, sealing P
tcrucible;
4), the Pt crucible of sealing is placed in Si-Mo rod stove, use Bridgman-Stockbarge method for growing crystal, the parameter of growing crystal is: furnace body temperature is 950 ~ 980 DEG C, inoculation temp is 820 ~ 860 DEG C, the thermograde of solid-liquid interface is 50 ~ 90 DEG C/cm, and crucible lowering speed is 0.2 ~ 2.0mm/h, after crystal growth terminates, with 20 ~ 80 DEG C/h decline furnace temperature to room temperature, obtain α-NaYF
4single crystal.
2. a kind of α-NaYF as claimed in claim 1
4the growth method of single crystal, is characterized in that described step 1) middle NaF, KF, YF
3raw material is 1: 1: 2.24 mixing in molar ratio, described step 4) in the thermograde of solid-liquid interface be 50 DEG C/cm.
3. a kind of α-NaYF as claimed in claim 1
4the growth method of single crystal, is characterized in that described step 1) middle NaF, KF, YF
3raw material is 2.40: 1: 3.40 mixing in molar ratio, described step 4) in the thermograde of solid-liquid interface be 90 DEG C/cm.
4. a kind of α-NaYF as claimed in claim 1
4the growth method of single crystal, is characterized in that described step 1) middle NaF, KF, YF
3purity be all greater than 99.99%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022232587A1 (en) * | 2021-04-30 | 2022-11-03 | University Of Washington | Porous cubic sodium yttrium fluoride gels, systems, methods, and materials thereof |
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