CN103436962A - Large-volume neodymium-doped yttrium vanadate crystal and preparation method thereof - Google Patents
Large-volume neodymium-doped yttrium vanadate crystal and preparation method thereof Download PDFInfo
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- CN103436962A CN103436962A CN2013103442930A CN201310344293A CN103436962A CN 103436962 A CN103436962 A CN 103436962A CN 2013103442930 A CN2013103442930 A CN 2013103442930A CN 201310344293 A CN201310344293 A CN 201310344293A CN 103436962 A CN103436962 A CN 103436962A
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Abstract
The invention discloses a large-volume neodymium-doped yttrium vanadate crystal, and the chemical formula of the large-volume neodymium-doped yttrium vanadate crystal is NdXY1-XVO4, wherein X is equal to 0.1-0.5%, the diameter of the crystal is 40-55 mm, and the isometric length of the crystal is 87 mm. The invention further discloses a preparation method of the crystal, and a melt pulling method is adopted to prepare the crystal. The large-volume neodymium-doped yttrium vanadate crystal and the preparation method of the large-volume neodymium-doped yttrium vanadate crystal have the following advantages that the growing thermal stress is further reduced through adjusting and optimizing the doping mixing ratio of the crystal and in the melt pulling method, through controlling the temperature gradient of the crystal by changing the thermal field, the pulling speed and the rotating speed. In addition, the crystal prepared through the melt pulling method is excellent in appearance and has few scattering particles and no constitutional supercooling phenomenon, and the internal quality of the crystal and the preparation process are guaranteed to be stable. The product crystal is large in volume, is high in the output laser power used on a laser device, and is well applicable to a high-power continuous laser device.
Description
Technical field
The present invention relates to the yttrium vanadate crystal field, in particular large volume Nd-doped yttrium vanadate crystal and preparation method thereof.
Background technology
Yttrium Orthovanadate (YV0
4) crystalline structure is tetragonal crystal, and the optical transparence of height is all arranged in the spectral range of 40-5000nm, can do polarizer and laser host material.The Laser emission cross section is large, is one of them of novel laser crystal material.Doping Nd
3+the crystal of ion has good applicability, Nd
3+the 4f energy level of ion is by 5s and 5p screening of nucleus, be subject to the impact of lattice less, quite long fluorescence lifetime and narrow live width are arranged, in visible region and near-infrared region, the large and wider absorption band of a series of uptake factors is arranged, fluorescence branching ratios are large, concentration of energy, there is sufficiently high laser transition terminal level on the ground state of being positioned at, therefore, at room temperature easily realize non-stop run, can realize 1064nm laser continuous operation.
Nd-doped yttrium vanadate (Nd
3+: YV0
4) crystal has larger stimulated emission cross section at the 1064nm place, is approximately 5 times of Nd:YAG crystal, reaches 25X10
-19/ cm
2; At the 808nm Absorber Bandwidth, being 21nm, is 2 times of Nd:YAG crystal; Having low threshold power, is half of Nd:YAG crystal.Improving constantly of the widespread use of crystal and the power of pumping, also more and more higher to the requirement of crystal.
In prior art, because the crystal growth has a series of technical requirements and device-restrictive, good Nd
3+: YV0
4crystal is mainly used in the LD Diode-pumped laser at present.Plain YV0
4the general diameter of crystal blank is 20-30mm, and length is 30-35mm.And require the high power laser of Output of laser power more than tens watts, and the corresponding increasing of its pump power, crystal bar volume, diameter and length also require corresponding increase.So existing Nd-doped yttrium vanadate (Nd
3+: YV0
4) crystal diameter and length little, the crystal volume is little, is not suitable for high power laser application.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, large volume Nd-doped yttrium vanadate crystal that a kind of crystal diameter is large, length is long, output rating is large, optical homogeneity is good and preparation method thereof is provided.
The present invention is achieved by the following technical solutions:
The invention provides a kind of large volume Nd-doped yttrium vanadate crystal, in described yttrium vanadate crystal, be mixed with Nd
3+ion, its chemical formula is:
Nd
XY
1-XVO
4
In formula, X=0.1-0.5%; Described crystal diameter is 40-55mm, and the electrical path length such as described crystal are 87mm.
The present invention also provides the preparation method of above-mentioned large volume Nd-doped yttrium vanadate crystal, adopts the preparation of melt crystal pulling method, comprises the steps:
(1) prepare raw material by chemical constitution, mix, seal in the latex mould of then packing into and pass through isostatic pressing;
(2) seed crystal is put into to seed rod;
(3) raw material of moulding is put into to the crucible of crystal furnace, mix up the temperature after vacuumize, be warmed up to 400 ℃, then be filled with high pure nitrogen protected;
(4) heat up, the raw material that makes moulding is all after fusing, the preheating seed crystal, and the crystal seed bar is the rotating speed rotation with 14-27 rev/min with seed crystal, starts slowly to descend seed crystal when temperature reaches 1800-1900 ℃, with bath surface, contacts to seed crystal;
(5) in the time of 1800-1900 ℃, constant temperature starts to lift seed crystal after 2-3 hour, start the crystal growth, shouldering, isodiametric growth, ending and cooling four-stage are passed through in the crystal growth successively, wherein seed crystal lifting speed is 2-4mm/h, the shouldering angle is 30-40 °, isodiametric growth when shouldering is 40-55mm to diameter, isodiametric growth length is 87mm, then ending heats up, after last slow cooling to 1000 ℃, per hour than the cooling rate that increases by 10 ℃ in last hour, to continue cooling, powered-down during to 400 ℃, carry out the nature cooling subsequently;
(6) after naturally being cooled to room temperature, take out crystal, obtain being mixed with the yag crystal rod of neodymium, cerium and chromium.
As the preparation method's of above-mentioned large volume Nd-doped yttrium vanadate crystal preferred implementation, described crystal furnace adopts the Medium-frequency Inverter induction heating.
As the preparation method's of above-mentioned large volume Nd-doped yttrium vanadate crystal preferred implementation, described crystal furnace adopts 99% aluminum oxide post-heater.
Attention: in crystal growing process, vanadium oxide easily volatilizees, and during batching, vanadium oxide is wanted corresponding increase, prevents the stress that uneven chemical components causes.Seed crystal will select does not have defective crystal.Adjust the crucible upper-lower position, find applicable axial-temperature gradient.
The present invention has the following advantages compared to existing technology:
Large volume Nd-doped yttrium vanadate crystal provided by the present invention and preparation method thereof, optimize the doping ratio of components of crystal by adjustment, and thereby the thermograde of controlling crystal in its melt crystal pulling method preparation method by changing Varied Temperature Field, change pull rate and rotating speed is controlled the speed of growth of crystal, and then reduced the growth thermal stresses, avoid crystal dislocation to increase and ftracture.Simultaneously, the axial-temperature gradient of major diameter crystal growth is than corresponding the reducing of axial-temperature gradient of minor diameter crystal growth, thus some defects that form in the minimizing crystal growing process.In addition, the crystal that this melt crystal pulling method prepares, good appearance, scattering particles are few, and, without the constitutional supercooling phenomenon, guarantee the crystals quality, thereby improve crystal optics quality and optical homogeneity, and stable preparation process.This product diameter is 40-55mm, etc. electrical path length, is 87mm, and the crystal volume is large, is used on laser apparatus Output of laser power high, and optical homogeneity is good, can well be applicable to the high power CW laser apparatus, has good application prospect.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment mono-
The present embodiment is the preferred embodiments of the present invention, and the present embodiment provides a kind of large volume Nd-doped yttrium vanadate crystal, in described yttrium vanadate crystal, is mixed with Nd
3+ion, its chemical formula is:
Nd
XY
1-XVO
4
In formula, X=0.3%; Described crystal diameter is 50mm, and the electrical path length such as described crystal are 87mm.
The present embodiment also provides the preparation method of above-mentioned large volume Nd-doped yttrium vanadate crystal, adopts the preparation of melt crystal pulling method, comprises the steps:
(1) prepare raw material by chemical constitution, mix, seal in the latex mould of then packing into and pass through isostatic pressing;
(2) seed crystal is put into to seed rod;
(3) raw material of moulding is put into to the crucible of crystal furnace, crystal furnace adopts the Medium-frequency Inverter induction heating, and adopts 99% aluminum oxide post-heater, vacuumizes after mixing up temperature, is warmed up to 400 ℃, then is filled with high pure nitrogen protected;
(4) heat up, the raw material that makes moulding is all after fusing, the preheating seed crystal, and the crystal seed bar is the rotating speed rotation with 20 rev/mins with seed crystal, starts slowly to descend seed crystal when temperature reaches 1850 ℃, with bath surface, contacts to seed crystal;
(5) in the time of 1850 ℃, constant temperature starts to lift seed crystal after 2 hours, start the crystal growth, shouldering, isodiametric growth, ending and cooling four-stage are passed through in the crystal growth successively, wherein seed crystal lifting speed is 3mm/h, the shouldering angle is 30-40 °, isodiametric growth when shouldering is 50mm to diameter, isodiametric growth length is 87mm, then ending heats up, after last slow cooling to 1000 ℃, per hour than the cooling rate that increases by 10 ℃ in last hour, to continue cooling, powered-down during to 400 ℃, carry out the nature cooling subsequently;
(6) after naturally being cooled to room temperature, take out crystal, obtain being mixed with the yag crystal rod of neodymium, cerium and chromium.
The crystal blank of above experiment growth cuts two, after the equal-diameter part polishing, with He-Ne Lasers, detects, and good appearance, scattering particles are in acceptability limit, without the constitutional supercooling phenomenon.
Embodiment bis-
The present embodiment provides a kind of large volume Nd-doped yttrium vanadate crystal, in described yttrium vanadate crystal, is mixed with Nd
3+ion, its chemical formula is:
Nd
XY
1-XVO
4
In formula, X=0.1%; Described crystal diameter is 40mm, and the electrical path length such as described crystal are 87mm.
The present embodiment also provides the preparation method of above-mentioned large volume Nd-doped yttrium vanadate crystal, adopts the preparation of melt crystal pulling method, comprises the steps:
(1) prepare raw material by chemical constitution, mix, seal in the latex mould of then packing into and pass through isostatic pressing;
(2) seed crystal is put into to seed rod;
(3) raw material of moulding is put into to the crucible of crystal furnace, crystal furnace adopts the Medium-frequency Inverter induction heating, and adopts 99% aluminum oxide post-heater, vacuumizes after mixing up temperature, is warmed up to 400 ℃, then is filled with high pure nitrogen protected;
(4) heat up, the raw material that makes moulding is all after fusing, the preheating seed crystal, and the crystal seed bar is the rotating speed rotation with 14 rev/mins with seed crystal, starts slowly to descend seed crystal when temperature reaches 1800 ℃, with bath surface, contacts to seed crystal;
(5) in the time of 1800 ℃, constant temperature starts to lift seed crystal after 2 hours, start the crystal growth, shouldering, isodiametric growth, ending and cooling four-stage are passed through in the crystal growth successively, wherein seed crystal lifting speed is 2mm/h, the shouldering angle is 30-40 °, isodiametric growth when shouldering is 40mm to diameter, isodiametric growth length is 87mm, then ending heats up, after last slow cooling to 1000 ℃, per hour than the cooling rate that increases by 10 ℃ in last hour, to continue cooling, powered-down during to 400 ℃, carry out the nature cooling subsequently;
(6) after naturally being cooled to room temperature, take out crystal, obtain being mixed with the yag crystal rod of neodymium, cerium and chromium.
The crystal blank of above experiment growth cuts two, after the equal-diameter part polishing, with He-Ne Lasers, detects, and good appearance, scattering particles only have minority, without the constitutional supercooling phenomenon.
Embodiment tri-
The present embodiment provides a kind of large volume Nd-doped yttrium vanadate crystal, in described yttrium vanadate crystal, is mixed with Nd
3+ion, its chemical formula is:
Nd
XY
1-XVO
4
In formula, X=0.2%; Described crystal diameter is 45mm, and the electrical path length such as described crystal are 87mm.
The present embodiment also provides the preparation method of above-mentioned large volume Nd-doped yttrium vanadate crystal, adopts the preparation of melt crystal pulling method, comprises the steps:
(1) prepare raw material by chemical constitution, mix, seal in the latex mould of then packing into and pass through isostatic pressing;
(2) seed crystal is put into to seed rod;
(3) raw material of moulding is put into to the crucible of crystal furnace, crystal furnace adopts the Medium-frequency Inverter induction heating, and adopts 99% aluminum oxide post-heater, vacuumizes after mixing up temperature, is warmed up to 400 ℃, then is filled with high pure nitrogen protected;
(4) heat up, the raw material that makes moulding is all after fusing, the preheating seed crystal, and the crystal seed bar is the rotating speed rotation with 17 rev/mins with seed crystal, starts slowly to descend seed crystal when temperature reaches 1825 ℃, with bath surface, contacts to seed crystal;
(5) in the time of 1825 ℃, constant temperature starts to lift seed crystal after 2 hours, start the crystal growth, shouldering, isodiametric growth, ending and cooling four-stage are passed through in the crystal growth successively, wherein seed crystal lifting speed is 2mm/h, the shouldering angle is 30-40 °, isodiametric growth when shouldering is 45mm to diameter, isodiametric growth length is 87mm, then ending heats up, after last slow cooling to 1000 ℃, per hour than the cooling rate that increases by 10 ℃ in last hour, to continue cooling, powered-down during to 400 ℃, carry out the nature cooling subsequently;
(6) after naturally being cooled to room temperature, take out crystal, obtain being mixed with the yag crystal rod of neodymium, cerium and chromium.
The crystal blank of above experiment growth cuts two, after the equal-diameter part polishing, with He-Ne Lasers, detects, and good appearance, scattering particles are in acceptability limit, without the constitutional supercooling phenomenon.
Embodiment tetra-
The present embodiment provides a kind of large volume Nd-doped yttrium vanadate crystal, in described yttrium vanadate crystal, is mixed with Nd
3+ion, its chemical formula is:
Nd
XY
1-XVO
4
In formula, X=0.4%; Described crystal diameter is 55mm, and the electrical path length such as described crystal are 87mm.
The present embodiment also provides the preparation method of above-mentioned large volume Nd-doped yttrium vanadate crystal, adopts the preparation of melt crystal pulling method, comprises the steps:
(1) prepare raw material by chemical constitution, mix, seal in the latex mould of then packing into and pass through isostatic pressing;
(2) seed crystal is put into to seed rod;
(3) raw material of moulding is put into to the crucible of crystal furnace, crystal furnace adopts the Medium-frequency Inverter induction heating, and adopts 99% aluminum oxide post-heater, vacuumizes after mixing up temperature, is warmed up to 400 ℃, then is filled with high pure nitrogen protected;
(4) heat up, the raw material that makes moulding is all after fusing, the preheating seed crystal, and the crystal seed bar is the rotating speed rotation with 24 rev/mins with seed crystal, starts slowly to descend seed crystal when temperature reaches 1850 ℃, with bath surface, contacts to seed crystal;
(5) in the time of 1850 ℃, constant temperature starts to lift seed crystal after 3 hours, start the crystal growth, shouldering, isodiametric growth, ending and cooling four-stage are passed through in the crystal growth successively, wherein seed crystal lifting speed is 3mm/h, the shouldering angle is 30-40 °, isodiametric growth when shouldering is 55mm to diameter, isodiametric growth length is 87mm, then ending heats up, after last slow cooling to 1000 ℃, per hour than the cooling rate that increases by 10 ℃ in last hour, to continue cooling, powered-down during to 400 ℃, carry out the nature cooling subsequently;
(6) after naturally being cooled to room temperature, take out crystal, obtain being mixed with the yag crystal rod of neodymium, cerium and chromium.
The crystal blank of above experiment growth cuts two, after the equal-diameter part polishing, with He-Ne Lasers, detects, and good appearance, scattering particles are in acceptability limit, without the constitutional supercooling phenomenon.
Embodiment five
The present embodiment provides a kind of large volume Nd-doped yttrium vanadate crystal, in described yttrium vanadate crystal, is mixed with Nd
3+ion, its chemical formula is:
Nd
XY
1-XVO
4
In formula, X=0.5%; Described crystal diameter is 55mm, and the electrical path length such as described crystal are 87mm.
The present embodiment also provides the preparation method of above-mentioned large volume Nd-doped yttrium vanadate crystal, adopts the preparation of melt crystal pulling method, comprises the steps:
(1) prepare raw material by chemical constitution, mix, seal in the latex mould of then packing into and pass through isostatic pressing;
(2) seed crystal is put into to seed rod;
(3) raw material of moulding is put into to the crucible of crystal furnace, crystal furnace adopts the Medium-frequency Inverter induction heating, and adopts 99% aluminum oxide post-heater, vacuumizes after mixing up temperature, is warmed up to 400 ℃, then is filled with high pure nitrogen protected;
(4) heat up, the raw material that makes moulding is all after fusing, the preheating seed crystal, and the crystal seed bar is the rotating speed rotation with 27 rev/mins with seed crystal, starts slowly to descend seed crystal when temperature reaches 1900 ℃, with bath surface, contacts to seed crystal;
(5) in the time of 1900 ℃, constant temperature starts to lift seed crystal after 3 hours, start the crystal growth, shouldering, isodiametric growth, ending and cooling four-stage are passed through in the crystal growth successively, wherein seed crystal lifting speed is 4mm/h, the shouldering angle is 30-40 °, isodiametric growth when shouldering is 55mm to diameter, isodiametric growth length is 87mm, then ending heats up, after last slow cooling to 1000 ℃, per hour than the cooling rate that increases by 10 ℃ in last hour, to continue cooling, powered-down during to 400 ℃, carry out the nature cooling subsequently;
(6) after naturally being cooled to room temperature, take out crystal, obtain being mixed with the yag crystal rod of neodymium, cerium and chromium.
The crystal blank of above experiment growth cuts two, after the equal-diameter part polishing, with He-Ne Lasers, detects, and good appearance, scattering particles only have minority, without the constitutional supercooling phenomenon.
Embodiment six
The present embodiment provides a kind of large volume Nd-doped yttrium vanadate crystal, in described yttrium vanadate crystal, is mixed with Nd
3+ion, its chemical formula is:
Nd
XY
1-XVO
4
In formula, X=0.5%; Described crystal diameter is 55mm, and the electrical path length such as described crystal are 87mm.
The present embodiment also provides the preparation method of above-mentioned large volume Nd-doped yttrium vanadate crystal, adopts the preparation of melt crystal pulling method, comprises the steps:
(1) prepare raw material by chemical constitution, mix, seal in the latex mould of then packing into and pass through isostatic pressing;
(2) seed crystal is put into to seed rod;
(3) raw material of moulding is put into to the crucible of crystal furnace, crystal furnace adopts the Medium-frequency Inverter induction heating, and adopts 99% aluminum oxide post-heater, vacuumizes after mixing up temperature, is warmed up to 400 ℃, then is filled with high pure nitrogen protected;
(4) heat up, the raw material that makes moulding is all after fusing, the preheating seed crystal, and the crystal seed bar is the rotating speed rotation with 25 rev/mins with seed crystal, starts slowly to descend seed crystal when temperature reaches 1900 ℃, with bath surface, contacts to seed crystal;
(5) start to lift seed crystal after during constant temperature 3 in the time of 1900 ℃, start the crystal growth, shouldering, isodiametric growth, ending and cooling four-stage are passed through in the crystal growth successively, wherein seed crystal lifting speed is 4mm/h, the shouldering angle is 30-40 °, isodiametric growth when shouldering is 55mm to diameter, isodiametric growth length is 87mm, then ending heats up, after last slow cooling to 1000 ℃, per hour than the cooling rate that increases by 10 ℃ in last hour, to continue cooling, powered-down during to 400 ℃, carry out the nature cooling subsequently;
(6) after naturally being cooled to room temperature, take out crystal, obtain being mixed with the yag crystal rod of neodymium, cerium and chromium.
The crystal blank of above experiment growth cuts two, after the equal-diameter part polishing, with He-Ne Lasers, detects, and good appearance, scattering particles are in acceptability limit, without the constitutional supercooling phenomenon.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. large volume Nd-doped yttrium vanadate crystal, is characterized in that, in described yttrium vanadate crystal, is mixed with Nd
3+ion, its chemical formula is:
Nd
XY
1-XVO
4
In formula, X=0.1-0.5%; Described crystal diameter is 40-55mm, and the electrical path length such as described crystal are 87mm.
2. the preparation method of large volume Nd-doped yttrium vanadate crystal as claimed in claim 1, is characterized in that, adopts the preparation of melt crystal pulling method, comprises the steps:
(1) prepare raw material by chemical constitution, mix, seal in the latex mould of then packing into and pass through isostatic pressing;
(2) seed crystal is put into to seed rod;
(3) raw material of moulding is put into to the crucible of crystal furnace, mix up the temperature after vacuumize, be warmed up to 400 ℃, then be filled with high pure nitrogen protected;
(4) heat up, the raw material that makes moulding is all after fusing, the preheating seed crystal, and the crystal seed bar is the rotating speed rotation with 14-27 rev/min with seed crystal, starts slowly to descend seed crystal when temperature reaches 1800-1900 ℃, with bath surface, contacts to seed crystal;
(5) in the time of 1800-1900 ℃, constant temperature starts to lift seed crystal after 2-3 hour, start the crystal growth, shouldering, isodiametric growth, ending and cooling four-stage are passed through in the crystal growth successively, wherein seed crystal lifting speed is 2-4mm/h, the shouldering angle is 30-40 °, isodiametric growth when shouldering is 40-55mm to diameter, isodiametric growth length is 87mm, then ending heats up, after last slow cooling to 1000 ℃, per hour than the cooling rate that increases by 10 ℃ in last hour, to continue cooling, powered-down during to 400 ℃, carry out the nature cooling subsequently;
(6) after naturally being cooled to room temperature, take out crystal, obtain being mixed with the yag crystal rod of neodymium, cerium and chromium.
3. the preparation method of large volume Nd-doped yttrium vanadate crystal as claimed in claim 2, is characterized in that, described crystal furnace adopts the Medium-frequency Inverter induction heating.
4. the preparation method of large volume Nd-doped yttrium vanadate crystal as claimed in claim 2, is characterized in that, described crystal furnace adopts 99% aluminum oxide post-heater.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198400A (en) * | 2015-10-12 | 2015-12-30 | 长春理工大学 | Medium-frequency induction sintering method for neodymium-doped yttrium aluminum garnet laser ceramic |
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| CN103074685A (en) * | 2013-02-01 | 2013-05-01 | 中山大学 | High concentration Nd-doped YAG laser crystal growth method |
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| US20080151954A1 (en) * | 2006-07-12 | 2008-06-26 | Ii-Vi Incorporated | Nd:YV04 laser crystal and method of growth and use thereof |
| CN101760774A (en) * | 2008-12-25 | 2010-06-30 | 福建福晶科技股份有限公司 | Post-heater for reduction of internal thermal stress of crystal grown in Czochralski method |
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| CN105198400A (en) * | 2015-10-12 | 2015-12-30 | 长春理工大学 | Medium-frequency induction sintering method for neodymium-doped yttrium aluminum garnet laser ceramic |
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