CN103290475B - GdAl3(BO3)4Crystal growth flux and GdAl3(BO3)4Crystal growth method - Google Patents
GdAl3(BO3)4Crystal growth flux and GdAl3(BO3)4Crystal growth method Download PDFInfo
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- CN103290475B CN103290475B CN201210047054.4A CN201210047054A CN103290475B CN 103290475 B CN103290475 B CN 103290475B CN 201210047054 A CN201210047054 A CN 201210047054A CN 103290475 B CN103290475 B CN 103290475B
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- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000004907 flux Effects 0.000 title 1
- 239000013078 crystal Substances 0.000 claims abstract description 101
- 229910001512 metal fluoride Inorganic materials 0.000 claims abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 15
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- 230000002457 bidirectional effect Effects 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 229910016036 BaF 2 Inorganic materials 0.000 claims description 2
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 2
- -1 SrF 2 Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000006184 cosolvent Substances 0.000 abstract description 4
- 238000002109 crystal growth method Methods 0.000 abstract 2
- 238000010583 slow cooling Methods 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 238000002156 mixing Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 230000003203 everyday effect Effects 0.000 description 7
- 238000007716 flux method Methods 0.000 description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 241001282153 Scopelogadus mizolepis Species 0.000 description 1
- WZGBFNDSTAFGNT-UHFFFAOYSA-N [Al+3].[Gd+3].[O-]B([O-])[O-].[O-]B([O-])[O-] Chemical compound [Al+3].[Gd+3].[O-]B([O-])[O-].[O-]B([O-])[O-] WZGBFNDSTAFGNT-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to a GdAl3(BO3)4Crystal growth co-solvent and GdAl3(BO3)4Crystal growth method, GdAl of the present invention3(BO3)4The crystal growth cosolvent is Al2O3-boride-lithiate-metal fluoride mixed system. GdAl by the present invention3(BO3)4Crystal growth co-solvent and GdAl3(BO3)4The crystal growth method can effectively reduce the crystal growth temperature, improve the crystal stability in the crystal growth process, improve the crystal growth quality and obtain large-size crystals.
Description
Technical field
The present invention relates to a kind of GdAl
3(BO
3)
4crystal growth fusing assistant and GdAl
3(BO
3)
4growing method, is specifically related to a kind of GdAl
3(BO
3)
4non-linear optic crystal growth fusing assistant and growing method thereof.
Background technology
Aluminum borate gadolinium GdAl
3(BO
3)
4crystal is a kind of non-linear optical crystal material found mid-term in 20th century.The advantages such as this crystal has that nonlinear factor is large, stable chemical performance, nonhygroscopic and hardness are large.Due to GdAl
3(BO
3)
4non-congruent compound, therefore GdAl
3(BO
3)
4the growth method of crystal is flux method.Flux method adopts fusing assistant system to mainly contain molybdate system etc.But molybdate fusing assistant system easily causes molybdenum to enter in lattice, has had a strong impact on crystal mass.Therefore be necessary that finding new suitable fusing assistant system grows excellent GdAl
3(BO
3)
4crystal.
Summary of the invention
The object of this invention is to provide a kind of GdAl
3(BO
3)
4crystal growth fusing assistant and GdAl
3(BO
3)
4growing method, to improve environment of crystal growth stability, obtains comparatively big scale monocrystalline.
GdAl of the present invention
3(BO
3)
4crystal growth fusing assistant is Al
2o
3-boride-lithiumation thing-metal fluoride mixed system;
Wherein, Al
2o
3: boride: lithiumation thing: the mol ratio of metal fluoride is (5 ~ 8): (2 ~ 4): (0.5 ~ 2): (0.0 ~ 1.5).Described Al
2o
3: boride: lithiumation thing: the mol ratio preferred (5 ~ 8) of metal fluoride: (2 ~ 4): (0.5 ~ 2): (0.5 ~ 1.5)
Wherein, described boride is B
2o
3or H
3bO
3; Described lithiumation thing is Li
2o or Li
2cO
3.
In addition, the preferred B of described boride
2o
3; The preferred Li of described lithiumation thing
2o.
In addition, described metal fluoride is monovalent metal fluorochemical or divalent metal fluoride.
In addition, described metal fluoride is MgF
2, CaF
2, SrF
2, BaF
2, one or more in LiF, NaF, KF.
The present invention also provides a kind of GdAl of described fusing assistant
3(BO
3)
4growing method, it comprises the steps:
(1) according to Gd
2o
3: fusing assistant be 1: 1 molar ratio mix after, be warming up to 1200 ~ 1300 DEG C of meltings, obtain grow material;
(2) after the complete melting of grower material, be cooled to 980 ~ 1100 DEG C, put into GdAl
3(BO
3)
4attempt seed crystal and find GdAl
3(BO
3)
4crystal growth temperature of saturation;
(3) GdAl is cooled to
3(BO
3)
4crystal growth temperature of saturation, puts into GdAl
3(BO
3)
4seed crystal grows, and growth is lowered the temperature with 0.1 ~ 2.0 DEG C/day with the speed rotating crystal of 20 ~ 40rpm simultaneously;
(4) after crystal growth to required yardstick, depart from growth material, be down to room temperature with 20 ~ 80 DEG C/h speed, obtain GdAl
3(BO
3)
4crystal.
Wherein, in described step (1), be that container takes up molten mass with platinum crucible.
In addition, in step (3), the direction putting into seed crystal is any direction.
In addition, in described step (3), Crystal Rotation can be single direction rotation or bidirectional rotation.
In addition, with GdAl
3(BO
3)
4attempt seed crystal and find GdAl
3(BO
3)
4crystal growth temperature of saturation, refers to GdAl
3(BO
3)
4seed crystal puts into cosolvent system, finds GdAl accurately
3(BO
3)
4crystal growth temperature numerical value, i.e. GdAl
3(BO
3)
4crystal growth temperature of saturation.Different seed crystals is in the solubility promoter of different ratio, its growth temperature of saturation is different, when putting into seed crystal higher than growth temperature of saturation, seed crystal melt-off can not normal growth, when putting into seed crystal lower than growth temperature of saturation, then crystal ramp becomes polycrystalline, can not get the result wanted, therefore, the present invention finds GdAl accurately to attempt seed crystal
3(BO
3)
4formal GdAl is put into again after crystal growth temperature
3(BO
3)
4seed crystal, makes it grow.
In addition, described GdAl
3(BO
3)
4seed crystal, without particular determination, namely can select commercially available prod, also can by following formula I at laboratory high temperature process heat.
Gd
2o
3+ 3Al
2o
3+ 8H
3bO
3=2GdAl
3(BO
3)
4+ 12H
2o formula I
In addition, described Crystal Rotation can be single direction rotation or bidirectional rotation, bidirectional rotation can be the bidirectional rotation rotated according to following swing circle: accelerate successively in a first direction to rotate, at the uniform velocity rotate, be rotated in deceleration and stop the rotation, afterwards, more in a second direction that is opposite the first direction accelerate successively to rotate, at the uniform velocity rotate, be rotated in deceleration and stop the rotation.In above-mentioned two-way choice, each party to rotational time preferably 1 ~ 10 minute, preferably 0.5 ~ 1 minute, bidirectional rotation interval.
Beneficial effect of the present invention:
1) effectively can reduce the growth temperature of crystal, make its growth temperature range between 980 ~ 1100 DEG C.
2) greatly can reduce the volatility of system, improve the stability of system in crystal growing process, prevent stray crystal from being formed, improve the speed of growth of crystal.
3) obviously can reduce the viscosity of solution, lower viscosity is conducive to solute transport, is easy to the growth of crystal and improves the growth quality of crystal.
4) a series of size larger high-quality GdAl3 (BO3) 4 monocrystalline can stably be grown.If use large size crucible, proper extension growth cycle, can also obtain corresponding larger sized single crystal.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
By 145.00gGd
2o
3, 203.92gAl
2o
3, 49.44gH
3bO
3, 14.78gLi
2cO
3with 24.92gMgF
2homogeneous phase mixing after grinding in agate mill, load in the platinum crucible of φ 80 × 70mm, put into monocrystal growing furnace, be heated to 1200 DEG C with the temperature rise rate of 70 DEG C/h, after above-mentioned crucible material is melted completely, Slow cooling temperature is to 960 DEG C.Then enter to attempt down seed crystal and seek saturation point temperature accurately.Control temperature is temperature of saturation, puts into the position of 5mm under seed crystal to solution surface, starts crystal growth.Seed rotation rate is per minute 40 turns, and rate of temperature fall is every day 0.2 ~ 2 DEG C.Terminate through 76 days crystal growth, 25mm place on crystal lift-off liquid level, be slow cooling to room temperature with 45 DEG C per hour, finally obtaining size is 10 × 10 × 16mm
3gdAl
3(BO
3)
4monocrystalline, crystal is transparent in inclusion.
Embodiment 2:
By 181.25gGd
2o
3, 254.90gAl
2o
3, 92.7gH
3bO
3, 18.47gLi
2cO
3in agate mill, Homogeneous phase mixing after grinding, loads in the platinum crucible of φ 90 × 80mm, puts into monocrystal growing furnace, be heated to 1300 DEG C with the temperature rise rate of 60 DEG C/h, make above-mentioned crucible material melt rear Slow cooling temperature completely to 980 DEG C.Then enter to attempt down seed crystal and seek saturation point temperature accurately.Control temperature is temperature of saturation, under enter the position of 30mm under formal seed crystal to solution surface, start crystal growth.Seed rotation rate is per minute 35 turns, and rate of temperature fall is 0.1 ~ 1.7 DEG C/day.Terminate through 50 days crystal growth, 20mm place on crystal lift-off liquid level, be slow cooling to room temperature with 20 DEG C per hour, finally obtaining size is 12 × 12 × 14mm
3gdAl
3(BO
3)
4monocrystalline.
Embodiment 3:
By 108.75gGd
2o
3, 244.70gAl
2o
3, 74.16gH
3bO
3, 33.25gLi
2cO
3with 11.71gCaF
2in agate mill, Homogeneous phase mixing after grinding, loads in the platinum crucible of φ 80 × 70mm, puts into monocrystal growing furnace, be heated to 1300 DEG C with the temperature rise rate of 30 DEG C/h, make above-mentioned crucible material melt rear Slow cooling temperature completely to 1020 DEG C.Then enter to attempt down seed crystal and seek saturation point temperature accurately.Control temperature is temperature of saturation, under enter the position of 5mm under formal seed crystal to solution surface, start crystal growth.Seed rotation rate is per minute 25 turns, and rate of temperature fall is every day 0.2 ~ 1.6 DEG C.Terminate through 68 days crystal growth, 30mm place on crystal lift-off liquid level, be slow cooling to room temperature with 60 DEG C per hour, finally obtaining size is 13 × 13 × 20mm
3gdAl
3(BO
3)
4monocrystalline.
Embodiment 4:
By 145.00gGd
2o
3, 244.70gAl
2o
3, 55.68gB
2o
3, 59.11gLi
2cO
3with 50.25gSrF
2in agate mill, Homogeneous phase mixing after grinding, loads in the platinum crucible of φ 90 × 80mm, puts into monocrystal growing furnace, be heated to 1250 DEG C with the temperature rise rate of 30 DEG C/h, make above-mentioned crucible material melt rear Slow cooling temperature completely to 1100 DEG C.Then enter to attempt down seed crystal and seek saturation point temperature accurately.Control temperature is temperature of saturation, under enter the position of 5mm under formal seed crystal to solution surface, start crystal growth.Seed rotation rate is per minute 25 turns, and rate of temperature fall is every day 0.4 ~ 2.0 DEG C.Terminate through 82 days crystal growth, 30mm place on crystal lift-off liquid level, be slow cooling to room temperature with 20 DEG C per hour, finally obtaining size is 16 × 16 × 22mm
3gdAl
3(BO
3)
4monocrystalline.
Embodiment 5:
By 145.00gGd
2o
3, 285.49gAl
2o
3, 83.52gB
2o
3, 29.56gLi
2cO
3with 35.06gBaF
2the rear Homogeneous phase mixing of grinding in agate mill is evenly mixed in after grinding in agate mill, load in the platinum crucible of φ 80 × 70mm, put into monocrystal growing furnace, be heated to 1250 DEG C with the temperature rise rate of 30 DEG C/h, make above-mentioned crucible material melt rear Slow cooling temperature completely to 980 DEG C.Then enter to attempt down seed crystal and seek saturation point temperature accurately.Control temperature is temperature of saturation, under enter the position of 5mm under formal seed crystal to solution surface, start crystal growth.Seed rotation rate is per minute 20 turns, and rate of temperature fall is every day 0.1 ~ 1.5 DEG C.Terminate through 66 days crystal growth, 25mm place on crystal lift-off liquid level, be slow cooling to room temperature with 30 DEG C per hour, finally obtaining size is 14 × 14 × 17mm
3gdAl
3(BO
3)
4monocrystalline.
Embodiment 6:
By 181.25gGd
2o
3, 254.90gAl
2o
3, 139.2gB
2o
3, 15.45gLi
2o
3homogeneous phase mixing after grinding in agate mill with 12.97gLiF, Homogeneous phase mixing after grinding in agate mill, load in the platinum crucible of φ 90 × 80mm, put into monocrystal growing furnace, 1300 DEG C are heated to the temperature rise rate of 50 DEG C/h, after above-mentioned crucible material is melted completely, Slow cooling temperature is to 1085 DEG C.Then enter to attempt down seed crystal and seek saturation point temperature accurately.Control temperature is temperature of saturation, under enter the position of 5mm under formal seed crystal to solution surface, start crystal growth.Seed rotation rate is per minute 30 turns, and rate of temperature fall is every day 0.3 ~ 1.6 DEG C.Terminate through 77 days crystal growth, 30mm place on crystal lift-off liquid level, be slow cooling to room temperature with 80 DEG C per hour, finally obtaining size is 17 × 17 × 18mm
3gdAl
3(BO
3)
4monocrystalline.
Embodiment 7:
By 126.88gGd
2o
3, 285.49gAl
2o
3, 86.56gH
3bO
3, 21.63gLi
2o
3homogeneous phase mixing after grinding in agate mill with 22.05gNaF, loads in the platinum crucible of φ 80 × 70mm, puts into monocrystal growing furnace, be heated to 1200 DEG C with the temperature rise rate of 50 DEG C/h, make above-mentioned crucible material melt rear Slow cooling temperature completely to 1030 DEG C.Then enter to attempt down seed crystal and seek saturation point temperature accurately.Control temperature is temperature of saturation, under enter the position of 5mm under formal seed crystal to solution surface, start crystal growth.Seed rotation rate is per minute 30 turns, and rate of temperature fall is every day 0.3 ~ 1.9 DEG C.Terminate through 84 days crystal growth, 30mm place on crystal lift-off liquid level, be slow cooling to room temperature with 70 DEG C per hour, finally obtaining size is 20 × 20 × 22mm
3gdAl
3(BO
3)
4monocrystalline.
Embodiment 8:
By 145.00gGd
2o
3, 244.70gAl
2o
3, 49.44gH
3bO
3, 49.44gLi
2o
3homogeneous phase mixing after grinding in agate mill with 23.24gKF, load in the platinum crucible of φ 80 × 70mm, put into monocrystal growing furnace, be heated to 1200 DEG C with the temperature rise rate of 50 DEG C/h, after above-mentioned crucible material is melted completely, Slow cooling temperature is to 1030 DEG C.Then enter to attempt down seed crystal and seek saturation point temperature accurately.Control temperature is temperature of saturation, under enter the position of 5mm under formal seed crystal to solution surface, start crystal growth.Seed rotation rate is per minute 30 turns, and rate of temperature fall is every day 0.3 ~ 1.9 DEG C.Terminate through 87 days crystal growth, 30mm place on crystal lift-off liquid level, be slow cooling to room temperature with 70 DEG C per hour, finally obtaining size is 24 × 24 × 28mm
3gdAl
3(BO
3)
4monocrystalline.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and replacement, these improve and replace and also should be considered as protection scope of the present invention.
Claims (9)
1. a GdAl
3(BO
3)
4the growth method of crystal, is characterized in that, comprises the steps:
(1) according to Gd
2o
3: fusing assistant is after the molar ratio of 1:1 mixes, and is warming up to 1200 ~ 1300 DEG C of meltings, obtains growing material;
(2) after the complete melting of grower material, be cooled to 980 ~ 1100 DEG C, put into GdAl
3(BO
3)
4attempt seed crystal and find GdAl
3(BO
3)
4crystal growth temperature of saturation;
(3) GdAl is cooled to
3(BO
3)
4crystal growth temperature of saturation, puts into GdAl
3(BO
3)
4seed crystal grows, and growth is lowered the temperature with 0.1 ~ 2.0 DEG C/day with the speed rotating crystal of 20 ~ 40rpm simultaneously;
(4) after crystal growth to required yardstick, depart from growth material, be down to room temperature with 20 ~ 80 DEG C/h speed, obtain GdAl
3(BO
3)
4crystal;
Described fusing assistant is Al
2o
3-boride-lithiumation thing-metal fluoride mixed system;
Wherein, Al
2o
3: boride: lithiumation thing: the mol ratio of metal fluoride is (5 ~ 8): (2 ~ 4): (0.5 ~ 2): (0.0 ~ 1.5).
2. method according to claim 1, is characterized in that, Al
2o
3: boride: lithiumation thing: the mol ratio of metal fluoride is (5 ~ 8): (2 ~ 4): (0.5 ~ 2): (0.5 ~ 1.5).
3. method according to claim 1 and 2, is characterized in that, described boride is B
2o
3or H
3bO
3; Described lithiumation thing is Li
2o or Li
2cO
3.
4. method according to claim 2, is characterized in that, described boride is B
2o
3; Described lithiumation thing is Li
2o.
5. method according to claim 1, is characterized in that, described metal fluoride is monovalent metal fluorochemical or divalent metal fluoride.
6. method according to claim 5, is characterized in that, described metal fluoride is MgF
2, CaF
2, SrF
2, BaF
2, one or more in LiF, NaF, KF.
7. method according to claim 1, is characterized in that, in described step (1), is that container takes up molten mass with platinum crucible.
8. method according to claim 1, is characterized in that, in step (3), the direction putting into seed crystal is any direction.
9. method according to claim 1, is characterized in that, in described step (3), Crystal Rotation can be single direction rotation or bidirectional rotation.
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|---|---|---|---|
| CN201210047054.4A CN103290475B (en) | 2012-02-27 | 2012-02-27 | GdAl3(BO3)4Crystal growth flux and GdAl3(BO3)4Crystal growth method |
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|---|---|---|---|
| CN201210047054.4A CN103290475B (en) | 2012-02-27 | 2012-02-27 | GdAl3(BO3)4Crystal growth flux and GdAl3(BO3)4Crystal growth method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101514481A (en) * | 2008-02-22 | 2009-08-26 | 中国科学院理化技术研究所 | BaAlBO3F2Flux growth method of crystal |
| CN101831706A (en) * | 2009-03-13 | 2010-09-15 | 中国科学院福建物质结构研究所 | Growth method of low ultraviolet absorption YA13(BO3)4 crystal |
| JP2011207633A (en) * | 2010-03-29 | 2011-10-20 | Sumitomo Osaka Cement Co Ltd | Cement clinker fluxing agent and method for producing cement clinker |
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2012
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101514481A (en) * | 2008-02-22 | 2009-08-26 | 中国科学院理化技术研究所 | BaAlBO3F2Flux growth method of crystal |
| CN101831706A (en) * | 2009-03-13 | 2010-09-15 | 中国科学院福建物质结构研究所 | Growth method of low ultraviolet absorption YA13(BO3)4 crystal |
| JP2011207633A (en) * | 2010-03-29 | 2011-10-20 | Sumitomo Osaka Cement Co Ltd | Cement clinker fluxing agent and method for producing cement clinker |
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