CN107723796B - A kind of method for growing strontium molybdate crystal - Google Patents
A kind of method for growing strontium molybdate crystal Download PDFInfo
- Publication number
- CN107723796B CN107723796B CN201710991667.6A CN201710991667A CN107723796B CN 107723796 B CN107723796 B CN 107723796B CN 201710991667 A CN201710991667 A CN 201710991667A CN 107723796 B CN107723796 B CN 107723796B
- Authority
- CN
- China
- Prior art keywords
- moo
- srmoo
- crystal
- growing
- flux
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910052712 strontium Inorganic materials 0.000 title description 4
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 title description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title description 2
- 150000002500 ions Chemical class 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 230000004907 flux Effects 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims 4
- 238000007716 flux method Methods 0.000 claims 2
- 229910002412 SrMoO4 Inorganic materials 0.000 abstract description 34
- 229910004619 Na2MoO4 Inorganic materials 0.000 abstract description 12
- 239000011684 sodium molybdate Substances 0.000 abstract description 12
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 9
- 229910020435 K2MoO4 Inorganic materials 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 5
- 229910015667 MoO4 Inorganic materials 0.000 abstract description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 22
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 description 8
- 229910000018 strontium carbonate Inorganic materials 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium (III) oxide Inorganic materials [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910018890 NaMoO4 Inorganic materials 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
-
- 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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/12—Salt solvents, e.g. flux growth
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/02—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of crystals, e.g. rock-salt, semi-conductors
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention provides a kind of for growing SrMoO4Crystal or active ions adulterate SrMoO4The method of crystal is prepared using top seed crystal flux growth metrhod, and fluxing agent used is Na 2MoO4+B2O3Or K2MoO4+B2O3Composite fluxing agent.In composite fluxing agent system, Na2MoO4Or K2MoO4With B2O3Molar ratio be 4:1, active ions Tm3+、Ho3+、Yb3+、Er3+Or Pr3+.Preparation SrMoO of the present invention4Crystal technology method, can be by SrMoO4The growth temperature of crystal reduces, while the volatility of melt system during the growth process, the growing environment of stable crystal can also be effectively reduced.
Description
Technical field
The contents of the present invention are a kind of for growing SrMoO4Crystal or active ions adulterate SrMoO4The side of crystal
Method is related to technical field of optoelectronic functional materials, more particularly, to preparing a kind of work that can be used as solid optically functional device
The artificial lens technical field of medium.
Background technique
Molybdate crystal due to having high density, good thermostabilization and irradiation stability, ideal flashing efficiency,
Make they photo-luminescent devices, solid-state laser, optical fiber, in terms of application it is more.
Alkali earth molybdates ReMoO4(Re=Mg, Sr) is a kind of important optical crystal matrix.SrMoO4It is the system
In important a member, it belongs to tetragonal crystal system, space group I41/ a, cell parameter are as follows: a=5.3897, c=12.0209
, z=4.In the crystal, Sr atom is eight-coordinate, and Mo atom is four-coordination.Every 6 SrO8Polyhedron is by sharing Sr-O
Polyhedral a line and form a Sr6O42Group connects each other together, SrMoO4Crystalline framework can regard this as
A little Sr6O42The cage structure that group is formed by connecting by way of sharing oxygen atom, MoO4Tetrahedron is filled in these caged
The gap of structure.
SrMoO4For congruent melting compound, melt temperature is 1460 DEG C.The crystal can be prepared by czochralski method,
Researcher is prepared for SrMoO using czochralski method4And it is doped with Tm3+、Ho3+、Yb3+、Er3+And Pr3+Equal active ions
SrMoO4Crystal.Meanwhile Chinese patent CN200810070582.5, CN200810070576.X, CN200810070568.5 points
Preparation doping Nd is not disclosed3+、Yb3+And Tm3+The SrMoO of ion4The preparation method of monocrystalline, what they were used is all czochralski method.
The melting point compound is higher, and the MoO in raw material3Saturated vapor pressure is lower, volatile so as to cause raw material deviation at high temperature
Standard stoichiometry ratio, so the SrMoO usually come out using Czochralski grown4Monocrystalline optical quality is to be improved.Therefore, existing
Some preparation SrMoO4There are the solutions of following two problems demand in the method for monocrystalline: 1, growth temperature is high;2, melt is in high temperature
Lower volatilization is serious.To solve above-mentioned two problems, Chinese patent CN200710009975.0 discloses a kind of improved czochralski method
For growing SrMoO4Monocrystalline.In the improved czochralski method, author introduces NaMoO4As fluxing agent, by SrMoO4Monocrystalline
Growth temperature is reduced to 1200 DEG C.But the growth temperature of the crystal is not still effectively reduced in this improved czochralski method,
NaMoO simultaneously4Addition there is no Essential Action to melt system volatility at high temperature is reduced.
Utilize K2MoO4SrMoO can be prepared as fluxing agent4Monocrystalline uses K2MoO4As fluxing agent and control its
Content in melt can also reduce SrMoO4The growth temperature of monocrystalline.But in whole system all it is in the molten state molybdenum
Hydrochlorate, the volatility of system are still very serious.
Summary of the invention
To solve SrMoO4The growth temperature height and melt faced in the existing preparation method of monocrystalline volatilizees seriously at high temperature
The problem of, the invention adopts the following technical scheme:
One kind is for growing SrMoO4The preparation method of crystal, which uses top seed crystal flux growth metrhod preparation, used
Fluxing agent is Na 2MoO4+B2O3Or K2MoO4+B2O3Composite fluxing agent.In above two composite fluxing agent system, Na2MoO4
Or K2MoO4With B2O3Ratio be 4:1(molar ratio).When with SrMoO4-Na2MoO4-B2O3System grows SrMoO4Crystal
When, solute SrMoO4Concentration be 25%-10%(molar ratio), crystal growth temperature section is 990 DEG C -880 DEG C, and rate of temperature fall is
0.5-5 DEG C/day, brilliant rotational speed rate is 5-60rpm;When with SrMoO4-K2MoO4-B2O3System grows SrMoO4When crystal, solute
SrMoO4Concentration be 25%-10%(molar ratio), crystal growth temperature section be 1050 DEG C -850 DEG C, rate of temperature fall 0.5-5
DEG C/day, brilliant rotational speed rate are 5-60rpm;
The SrMoO prepared using the technical method4Crystal, crystal parameters are as follows: tetragonal crystal system, space group
For I41/ a, cell parameter are as follows: a=5.3897, c=12.0209, z=4;
SrMoO is prepared using the technical method4When crystal, it can according to need and adulterate active ions thereto, such as Tm3+、
Ho3+、Yb3+、Er3+And Pr3+Ion etc., the Sr in these active ions replacement lattices2+, to prepare active ions doping
SrMoO4Crystal, wherein the doping of active ions is 1-10 at.%;
In above-mentioned technical method, SrMoO4Raw material be SrCO3And MoO3, K2MoO4Raw material be K2CO3And MoO3,
Na2MoO4Raw material be Na2CO3And MoO3, B2O3Then derive from H3BO3.At high temperature, above-mentioned raw materials are according to following chemical equation
Formula is reacted:
Na2CO3+MoO3= Na2MoO4+CO2↑
K2CO3+MoO3= K2MoO4+CO2↑
SrCO3+MoO3=SrMoO4 +CO2↑
2H3BO3=3H2O↑+B2O3
In the above preparation method, B2O3Introducing be necessary. B2O3Introducing can effectively improve melt system
Viscosity reduces the volatilization of melt system and entire melt is made to become thoroughly bright, is very beneficial for the molten of stable crystal growth
Body environment.In order to illustrate B2O3Introducing be able to suppress the volatility of melt system, we devise one group of comparative test: we
Choose SrMoO4-Na2MoO4-B2O3And SrMoO4-Na2MoO4System carries out thermogravimetric analysis, and raw materials used is AR grades of SrCO3、
Na2CO3、MoO3And H3BO3, the model SDT Q600 V8.2 Build 100 of thermogravimetric analyzer.SrMoO4-Na2MoO4-B2O3
System according to three 1:1:1 molar ratio ingredient 15mg, SrMoO4-Na2MoO4System according to the two 1:1 molar ratio ingredient
15mg.It tests two systems and rises to the variation of 900 DEG C of system gross masses with the raised relationship of temperature, heating rate 10 from room temperature
DEG C/minute, 100 minutes are kept the temperature at 900 DEG C.Test result is as depicted in figs. 1 and 2.
As shown in Figure 1, two fluxing agent systems are before 500 DEG C with the H in raw material2O、H3BO3、SrCO3And Na2CO3
Participation physical-chemical reaction decompose, the quality of system will appear several places and die-offs or reduce in ladder shape.Specifically,
SrMoO4-Na2MoO4Have in system raw material and holds evaporable H2The O and SrCO for being easy reaction decomposition3And Na2CO3, in temperature-rise period
In have following variation: from room temperature to 71 DEG C, since the evaporation system TG of water has dropped to 96% from 100%;From 71 DEG C to 330 DEG C,
Due to Na2CO3With MoO3It reacts, generates CO2, along with dehydration is continued, system TG is down to 84%;It is warming up to from 482 DEG C
490 DEG C, due to SrCO3With MoO3It reacts, generates CO2, system gross mass accounts for material quality and becomes 82.8% from 83%.
And the SrMoO before 500 DEG C4-Na2MoO4-B2O3System is from 71 DEG C to 330 DEG C in addition to there is Na2CO3With
MoO3It reacts and generates CO2Except, there are also H3BO3The process of dehydration.Two individuals tie up to gross mass base between 500 DEG C to 800 DEG C
Originally it remains unchanged.After 800 DEG C, as the temperature rises, SrMoO4-Na2MoO4-B2O3Gross mass it is nearly constant constant, and
SrMoO4-Na2MoO4The gross mass of system is then also decreasing.
Fig. 2 is SrMoO4-Na2MoO4-B2O3And SrMoO4-Na2MoO4The thermogravimetric of holding stage after system is warming up to 900 DEG C
Analysis, constant in system is SrMoO in 900 DEG C of holdings 100 minutes4-Na2MoO4-B2O3System gross mass is down to by 100%
98.6%, and SrMoO4-Na2MoO4System gross mass is down to 97.4% by 100%, due to B2O3Presence and reduce system melt
Volatilization.The results show of Fig. 1 and Fig. 2, B2O3Apparent inhibiting effect can be played to the volatility of system.
By SrMoO4Crystal or the SrMoO of active ions doping4The Solid-state Optics device system that crystal is used to prepare,
The Solid-state Optics device system can be used for particle detection, laser device, spectroscopy device, biomedicine or military field.
Beneficial effects of the present invention
Preparation SrMoO of the present invention4Crystal technology method, can be by SrMoO4The growth temperature of crystal reduces, together
When the volatility of melt system during the growth process, the growing environment of stable crystal can also be effectively reduced.
Detailed description of the invention
Fig. 1 is SrMoO4-Na2MoO4-B2O3And SrMoO4-Na2MoO4System temperature rise period thermogravimetric map;
Fig. 2 is SrMoO4-Na2MoO4-B2O3And SrMoO4-Na2MoO4The heat of holding stage after system is warming up to 900 DEG C
Multigraph spectrum;
Fig. 3 is the resulting SrMoO of embodiment 14Monocrystalline;
Fig. 4 is the resulting SrMoO of embodiment 24Monocrystalline;
Fig. 5 is the resulting Tm of embodiment 33+:SrMoO4Monocrystalline;
Fig. 6 is embodiment 1,2 resulting SrMoO4Monocrystalline and the resulting Tm of embodiment 33+:SrMoO4The XRD spectrum of monocrystalline;
Fig. 7 is 3 gained Tm of embodiment3+:SrMoO4Room temperature absorption spectrum;
Fig. 8 is 3 gained Tm of embodiment3+:SrMoO4Crystal Room temperature PL spectrum.
Specific embodiment
The present invention is further illustrated by the following examples, but protection scope of the present invention is not limited to following reality
Apply example
Embodiment 1:
According to SrMoO4-Na 2MoO4-B2O3=1:4:1(molar ratio), system gross weight is 150 grams of specification after melting, weigh
MoO3、SrCO3、Na2CO3And H3BO3Equal raw materials, the purity of above-mentioned raw materials are that analysis is pure.Platinum is put into after raw material is fully ground
Golden crucible is placed in molten salt furnace, is warming up to powder fine melt, and keeps the temperature 24 hours after fine melt, and a platinum wire is wrapped in corundum seed
The top of crystalline style is used as seed crystal, is then slowly drop down to ullage until contacting with liquid level.It quickly cools the temperature to molten
Or more after cooled down 7 days with the speed of 5 DEG C/d again, then lift seed rod, room temperature be annealed to the rate of 20 DEG C/h, is obtained
SrMoO4Polycrystalline cuts out the preferable seed crystal of quality in polycrystalline, and remaining polycrystal material is put into crucible and melts recycling.
In the second wheel crystal growing process, the saturation point of system is first found, is 985 DEG C.In the temperature by seed crystal immersed in liquid level hereinafter,
The rate of temperature fall of crystal growth be 1 DEG C/for 24 hours, brilliant rotational speed rate be 30rpm, growth time be 30 days, annealing rate be 15 DEG C/h
800 DEG C are down to, 20 DEG C/h is down to 600 DEG C, and 40 DEG C/h is down to 400 DEG C, is then quickly down to room temperature.With this growth technique, we are obtained
The more excellent SrMoO of quality is arrived4Monocrystalline.
Embodiment 2:
According to SrMoO4- K2MoO4-B2O3=1:4:1(molar ratio), system gross weight is 180 grams of specification after melting, weigh
MoO3、SrCO3、K2CO3And H3BO3Equal raw materials, the purity of above-mentioned raw materials are that analysis is pure.Platinum is put into after raw material is fully ground
Crucible is placed in molten salt furnace, is warming up to powder fine melt, and keeps the temperature 24 hours after fine melt, and a platinum wire is wrapped in corundum seed crystal
The top of bar is used as seed crystal, is then slowly drop down to ullage until contacting with liquid level.Quickly cool the temperature to fusing point
Cooled down 3 days with the speed of 5 DEG C/d again after above, then lifts seed rod, room temperature is annealed to the rate of 10 DEG C/h, is obtained
SrMoO4Polycrystalline cuts out the preferable seed crystal of quality in polycrystalline, and remaining polycrystal material is put into crucible and melts recycling.
In the second wheel crystal growing process, the saturation point of system is first found, is 948 DEG C.In the temperature by seed crystal immersed in liquid level hereinafter,
The rate of temperature fall of crystal growth be 2 DEG C/for 24 hours, brilliant rotational speed rate be 20rpm, growth time be 10 days, annealing rate be 15 DEG C/h
It is down to room temperature.With the more excellent SrMoO of the available quality of this growth technique4Monocrystalline.
Embodiment 3:
According to SrMoO4-Na2MoO4-B2O3=1:4:1(molar ratio), Tm3+Account for SrMoO4Amount be 10at.%, system melt
Gross weight is 200 grams of specification later, and weighs raw material according to following reaction formula:
(1-x) SrCO3+(x/3)Tm2O3+ MoO3=Sr1-xTm2x/3MoO4+(1-x)CO2↑
Wherein, Tm2O3Purity be 99/99%.Using seed crystal obtained in embodiment 1, in 985 DEG C of (saturations of the system
Point) when by seed crystal immersed in liquid level hereinafter, and according to rate of temperature fall be 1 DEG C/for 24 hours, brilliant rotational speed rate be 30rpm technique, by 30
The second best in quality Tm can be obtained in it growth cycle3+Ion doping SrMoO4(Tm3+:SrMoO4) monocrystalline.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (4)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710991667.6A CN107723796B (en) | 2017-10-23 | 2017-10-23 | A kind of method for growing strontium molybdate crystal |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710991667.6A CN107723796B (en) | 2017-10-23 | 2017-10-23 | A kind of method for growing strontium molybdate crystal |
Publications (2)
Publication Number | Publication Date |
---|---|
CN107723796A CN107723796A (en) | 2018-02-23 |
CN107723796B true CN107723796B (en) | 2019-05-10 |
Family
ID=61212334
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201710991667.6A Active CN107723796B (en) | 2017-10-23 | 2017-10-23 | A kind of method for growing strontium molybdate crystal |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107723796B (en) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101457398A (en) * | 2007-12-11 | 2009-06-17 | 中国科学院福建物质结构研究所 | Ytterbium sodium ion double doped strontium molybdate laser crystal and preparation method thereof |
CN101498045A (en) * | 2008-01-31 | 2009-08-05 | 中国科学院福建物质结构研究所 | Ytterbium strontium molybdate doped tunable laser crystal |
CN102851029A (en) * | 2012-06-30 | 2013-01-02 | 四川师范大学 | Na4-3xEux(WO4)2-y(MoO4)y series fluorescent microcrystals and preparation method of chemical solution thereof |
-
2017
- 2017-10-23 CN CN201710991667.6A patent/CN107723796B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101457398A (en) * | 2007-12-11 | 2009-06-17 | 中国科学院福建物质结构研究所 | Ytterbium sodium ion double doped strontium molybdate laser crystal and preparation method thereof |
CN101498045A (en) * | 2008-01-31 | 2009-08-05 | 中国科学院福建物质结构研究所 | Ytterbium strontium molybdate doped tunable laser crystal |
CN102851029A (en) * | 2012-06-30 | 2013-01-02 | 四川师范大学 | Na4-3xEux(WO4)2-y(MoO4)y series fluorescent microcrystals and preparation method of chemical solution thereof |
Also Published As
Publication number | Publication date |
---|---|
CN107723796A (en) | 2018-02-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP3620555B1 (en) | Compound of cesium fluorooxoborate, non-linear optical crystal of cesium fluorooxoborate, preparation method therefor and use thereof | |
CN102251281B (en) | Process for producing Zno single crystal according to method of liquid phase growth | |
CN102076892A (en) | Doped low temperature phase BaB204 single crystal, the manufacturing method thereof and wave changing elements therefrom | |
CN101565192B (en) | Methods for preparing anhydrous lithium iodide and scintillation crystal doped with lithium iodide | |
CN101435109B (en) | Fluxing agent growth method of boron phosphate single crystal | |
US10564514B1 (en) | Nonlinear optical crystal of cesium fluorooxoborate, and method of preparation and use thereof | |
CN107723796B (en) | A kind of method for growing strontium molybdate crystal | |
CN107761168B (en) | Mix ytterbium sodium calcium-lithium-niobium garnet crystal, preparation method and application | |
CN101092746B (en) | Alterovalent ion synergistically doped high light yield lead tungstate crystal and its preparation method | |
CN114250514B (en) | Flux for beta-gallium trioxide crystal growth and crystal growth method based on flux | |
Ivanov et al. | Novel solvents for the single crystal growth of germanate phases by the flux method | |
CN101935879B (en) | Ytterbium bismuth double-doped lead tungstate crystal and preparation method thereof | |
CN102912435A (en) | Preparation method of self-activation laser crystal phosphoric acid trisneodymium | |
DE1667604B1 (en) | PROCESS FOR THE PRODUCTION OF CRYSTALLINE CADMIUM TELLURIDE | |
CN208776874U (en) | A kind of crucible for growing lithium niobate crystal with near stoichiometric ratio | |
CN114262933A (en) | Growth method of boron 10-LBO crystal | |
CN102485976A (en) | Method and device for near stoichiometric lithium niobate single crystal growth | |
CN107059109A (en) | Al-doped CsLiB6O10Crystal growth fluxing agent and crystal growth method | |
CN107541781A (en) | A kind of method for being used to grow borosilicic acid lanthanum crystal | |
CN103031604A (en) | Nonlinear optical crystal rubidium calcium fluorine carbonate | |
CN111621848A (en) | Compound tin boron oxygen bromine, tin boron oxygen bromine nonlinear optical crystal, preparation method and application | |
CN1155742C (en) | Melt Growth Method of Sodium Borophosphate Crystal | |
CN111379014A (en) | A kind of flux for crystal growth and crystal growth method | |
CN106958041B (en) | A kind of xTeO2·P2O5(x=2,4) preparation method and preparation facilities of crystal | |
CN103290475B (en) | GdAl3(BO3)4Crystal growth flux and GdAl3(BO3)4Crystal growth method |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |