CN109097820A - A kind of preparation method and application for exempting to process sheet laser crystal - Google Patents
A kind of preparation method and application for exempting to process sheet laser crystal Download PDFInfo
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- CN109097820A CN109097820A CN201811038334.2A CN201811038334A CN109097820A CN 109097820 A CN109097820 A CN 109097820A CN 201811038334 A CN201811038334 A CN 201811038334A CN 109097820 A CN109097820 A CN 109097820A
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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
- 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
- C30B9/06—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using as solvent a component of the crystal composition
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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
- C30B29/14—Phosphates
Abstract
The invention belongs to laser materials and laser technology field, are related to a kind of preparation method and application for exempting to process sheet laser crystal, by Re2O3With PbHPO4Mixing is put into platinum crucible, wherein Re is Nd and Y, it or is Nd and Lu, when crystal growth, elder generation is from room temperature to 1250 DEG C and keeps the temperature for 24 hours, starts cooling growth after solution-stabilized, the power supply that platinum crucible is closed after being down to 900 DEG C makes it be naturally cooling to room temperature, it is finally impregnated 2 days with boiling concentrated nitric acid, crystal is separated from fluxing agent, obtain sheet laser crystal；The sheet laser crystal of preparation can doping concentration it is high, gain is big, and fluorescence lifetime is long, and thermal conductivity is high, and light injury threshold is high, readily available low pumping threshold, high efficiency, high power laser light output；And convenient for combining with passive Q-adjusted element or nonlinear optical element, to obtain pulse or visible, ultraviolet laser, miniaturization, at low cost, the service life is long, easy to carry, easy-to-use, has broad prospect of application.
Description
Technical field:
The invention belongs to laser materials and laser technology field, are related to a kind of preparation method for exempting to process sheet laser crystal
And application.
Background technique
Laser technology has been grown rapidly since appearance as one of greatest invention of twentieth century, is produced to contemporary society
Great influence is given birth to.The development of laser radar, laser weapon, laser processing, the technologies such as laser medicine proposes laser material
New requirement, promotes continuous exploration of the people to new pattern laser material.Laser crystal is a kind of common Solid State Laser Jie
Matter has very extensive application.The composition of laser crystal mainly includes doping with rare-earth ions and host material.Solid state laser
Efficient, high-power output is obtained, the performance of laser crystal is most important.The preparation flow of laser crystal is general at present are as follows: root
According to the characteristic of different crystal, obtained using corresponding growing method (such as czochralski method, flux growth metrhod, Bridgman-Stockbarger method etc.) blocky brilliant
Body is cut, shaping after crystal orientation along the direction and thickness needed, then rough polishing, essence throwing, plated film, last ability
It uses, whole process technique is cumbersome, and elapsed time is long, at high cost, it may be said that valence of the processing cost in laser crystal device
Important proportion is occupied in lattice, sometimes the even more than cost of material itself, and for the quartz crystal device of chip shape,
Required precision is high, and risk of breakage is big, and yield rate is low, and material loss is more, and (for commonly using process equipment at present, one knife of cutting can be damaged
Consume the crystal of about 0.25mm thickness), processing cost remains high for a long time.
Summary of the invention
It is an object of the invention to overcome disadvantage of the existing technology, design provides one kind and exempts to process sheet laser crystal
Preparation method and application.
To achieve the goals above, present invention preparation exempts to process the detailed process of sheet laser crystal are as follows:
(1) by Re2O and PbHPO4Be put into platinum crucible with molar ratio 1:23 mixing, wherein Re is Nd and Y, or for Nd and
Lu, neodymium ion doped concentration are 0.05-50at.%；PbHPO4Pb is resolved into platinum crucible2P2O7, a part of Pb2P2O7With
Re2O3Reaction generates RePO4, another part is as fluxing agent, specific chemical reaction are as follows:
Pb2P2O7+Re2O3=2RePO4+2PbO；
(2) when crystal growth, 1250 DEG C is first warming up to as early as possible from room temperature and is kept the temperature for 24 hours, start cooling life after solution-stabilized
Long, rate of temperature fall is 1 DEG C/h；After being down to 900 DEG C, crystal is no longer grown substantially, and the power supply for being then turned off platinum crucible makes it certainly
It so is cooled to room temperature, is finally impregnated 2 days with the concentrated nitric acid of the mass fraction 65%-68% of boiling, crystal is divided from fluxing agent
It separates out and, obtain the surface depth of parallelism, flatness, highly polished sheet laser crystal.
Sheet laser crystal prepared by the present invention is the rare earth doped orthophosphates crystal of neodymium, for cubic zircon structure, molecule
Formula is Nd:APO4, wherein A is element Y or Lu.
Crystal prepared by the present invention is fast in the growth of [001] direction, and in [100] direction, growth is slow, and easily high-volume obtains table.
Sheet laser crystal prepared by the present invention can be used for all solid state laser, and all solid state laser is along its yuan of optical path direction
Part puts in order successively are as follows: pumping source, laser focusing system, pumping end mirror, sheet laser crystal, output end mirror, wherein pumping
Pu source is semiconductor laser, and launch wavelength is directed at the absorption bands of sheet laser crystal, and the laser of pumping source transmitting passes through
Laser focusing system is incident in sheet laser crystal, pump be coated on end mirror it is high to pump light thoroughly, it is high to operating laser anti-
Deielectric-coating, sheet laser crystal are primary, the neodymium-doped rare earth orthophosphates crystal without any processing, plated film, output end mirror
It is coated with the deielectric-coating penetrated to operating laser part.
Compared with prior art, the present invention having the advantage that first is that obtained neodymium-doped rare earth orthophosphates crystal has
Flake-like shape, optical quality is high, can directly meet laser application needs without any processing, plated film, to make the production time
It is greatly lowered with production cost；Second is that flat crystal have can doping concentration it is high, gain is big, and fluorescence lifetime is long, and thermal conductivity is high,
The advantages that light injury threshold is high, readily available low pumping threshold, high efficiency, high power laser light output；Third is that the flake crystalline of preparation
Volumetric laser, to obtain pulse or visible, ultraviolet laser, has convenient for combining with passive Q-adjusted element or nonlinear optical element
Miniaturization, the advantages that at low cost, the service life is long, easy to carry, easy-to-use, in scientific research, electronics, biology, medical treatment, environmental monitoring etc.
Field has broad prospect of application.
Detailed description of the invention:
Fig. 1 is the principle schematic diagram of all solid state laser of the present invention.
Specific embodiment:
Below by embodiment, the invention will be further described.
Embodiment 1:
The present embodiment preparation adulterates 1.2at.%, having a size of 3 × 2 × 0.6mm3Nd:YPO4Native transistors thin slice, specifically
Preparation process are as follows: weigh 2.6 grams of Y2O3, 80 grams of PbHPO4With 0.0234 gram of Nd2O3Mixing is put into platinum crucible, first as early as possible from room temperature
It is warming up to 1250 DEG C and keeps the temperature for 24 hours, start cooling growth after solution-stabilized, rate of temperature fall is 1 DEG C/h；After being down to 900 DEG C, then
The power supply for closing platinum crucible makes it be naturally cooling to room temperature, finally impregnates 2 with boiling concentrated nitric acid (mass fraction 65%-68%)
It, crystal is separated from fluxing agent, obtains the surface depth of parallelism, flatness, highly polished sheet laser crystal.
The present embodiment is by the Nd:YPO of preparation4Native transistors thin slice is directly placed into after 1.06 mum laser resonant cavities, can
To obtain the output power of 2W or more, slope efficiency and light light conversion efficiency respectively reach 56.4%, 53%；It is directly placed into 1.34
After mum laser resonant cavity, the output power of 800mW or more can be obtained, slope efficiency and light light conversion efficiency respectively reach
28.2%, 26%.
Embodiment 2:
The present embodiment exempts from processing neodymium-doped 1.2at.% orthophosphoric acid yttrium crystal (YPO for preparation4) continuous for 1.06 microns
Wave all solid state laser, along putting in order successively for optical path direction element are as follows: pumping source, pumping end mirror, swashs at laser focusing system
Luminescent crystal, output end mirror, wherein laser crystal is the neodymium-doped rare earth orthophosphates crystal for exempting from processing, crystal thickness 0.1-2mm；
Pumping source is the fiber coupling output semiconductor laser of center wavelength 808nm；Pumping end mirror is coated with high to 800-815nm light
Thoroughly, to the high anti-deielectric-coating of 1040-1080nm light；Output end mirror is coated with the deielectric-coating penetrated to 1040-1080nm light part, thoroughly
The rate T of mistake can change between 0.5% to 60%, and the transmitance of optimization is 5% to 20%；It pumps end mirror and output end mirror is non-
Very close to the both ends of laser crystal, the pump light of pumping source transmitting is irradiated to laser crystal by focusing system and pumping end mirror
On, laser crystal generates 1.06 microns of continuous wave near-infrared laser, in pumping end mirror and exports in the resonant cavity that end mirror is constituted
Oscillation, and exported in output end mirror side.
The present embodiment saves crystal using the laminar neodymium-doped rare earth orthophosphates crystal for exempting from processing as working media
Processing cost and process time, and flake-like crystals are advantageously implemented cramped construction and the miniaturization of laser.
Embodiment 3:
The present embodiment will exempt from processing and mix 1.2at.% orthophosphoric acid yttrium crystal (YPO4) all solid state for 1.34 microns of continuous waves
Laser, along putting in order successively for all solid state laser optical path direction element are as follows: pumping source, laser focusing system, pumping end
Mirror, laser crystal, output end mirror, wherein laser crystal is the neodymium-doped rare earth orthophosphates crystal for exempting from processing, and crystal thickness is
0.1-2mm；Pumping source is the fiber coupling output semiconductor laser of center wavelength 808nm；Pumping end mirror is coated with to 800-
High thoroughly, anti-to the 1.32-1.36 light height deielectric-coating of 815nm, 1040-1080nm light；Output end mirror is coated with to 1040-1080nm light
The high deielectric-coating penetrated thoroughly, to 1.32-1.36 light part, transmitance T can change between 0.5% to 60%, optimization it is saturating
Crossing rate is 2% to 10%；End mirror and output end mirror are pumped very close to the both ends of laser crystal, the pumping of half pumping source transmitting
Light is irradiated on laser crystal by focusing system and pumping end mirror, due to the special designing of hysteroscope membrane system, can effectively be inhibited
The biggish 1.06 mum laser oscillation of emission cross section, and promote the oscillation and effectively output of 1.34 microns of continuous wave lasers.
Embodiment 4:
The present embodiment will exempt to process neodymium-doped 1.2at.% orthophosphoric acid yttrium crystal (YPO4) it is used for 1.06 microns of complete solid state pulses
Laser, along putting in order successively for complete solid state pulse laser light path directional element are as follows: pumping source, laser focusing system, pump
Pu end mirror, laser crystal, passive Q-adjusted crystal, output end mirror, laser crystal are the neodymium-doped rare earth orthophosphates crystal for exempting from processing,
Crystal thickness is 0.1-2mm；Passive Q-adjusted crystal is Cr:YAG, and cut direction is (111), and length 0.2-2mm is micro- 1.06
The initial transmission of rice can be 50~99%, and the initial transmission of optimization is 75~92%, both ends be coated with 1.06 microns it is anti-reflection
Deielectric-coating；Pumping source is the fiber coupling output semiconductor laser of center wavelength 808nm；Pumping end mirror is coated with to 800-
High thoroughly, anti-to the 1040-1080nm light height deielectric-coating of 815nm light；Output end mirror is coated with to 1040-1080nm light part transmission
Deielectric-coating；End mirror is pumped close to laser crystal, exports end mirror close to passive Q-adjusted crystal, the pump light of pumping source transmitting is by poly-
Burnt system and pumping end mirror are irradiated on laser crystal, and laser crystal generates 1.06 microns of near-infrared laser, through passive Q-adjusted crystalline substance
After body modulation, 1.06 microns of pulse laser is exported in output end mirror side.
Embodiment 5:
The present embodiment will exempt to process neodymium-doped 1.2at.% orthophosphoric acid yttrium crystal (YPO4) it is used for 0.53 micron of all solid state green light
Laser, along putting in order successively for optical path direction element are as follows: pumping source, laser focusing system, pumping end mirror, laser crystal,
Frequency-doubling crystal, output end mirror, wherein laser crystal is the neodymium-doped rare earth orthophosphates crystal for exempting from processing, crystal thickness 0.1-
2mm；Frequency-doubling crystal is KTP, and cut direction is (90 °, 23.6 °), and length 5mm, 1.06,0.53 microns of anti-reflection films are plated at both ends；Pump
Pu source is the fiber coupling output semiconductor laser of center wavelength 808nm；Pumping end mirror be coated with it is high to 800-815nm light thoroughly,
To the high anti-deielectric-coating of 520-540,1040-1080nm light；Output end mirror is coated with the anti-, 520-540nm high to 1040-1080nm high
Saturating deielectric-coating；End mirror is pumped close to laser crystal, exports end mirror close to frequency-doubling crystal, the pump light of pumping source transmitting is by poly-
Burnt system and pumping end mirror are irradiated on laser crystal, and laser crystal generates 1.06 microns of near-infrared laser, through nonlinear optical
After learning crystal KTP frequency multiplication, 0.53 micron of green laser is exported in output end mirror side.
Embodiment 6:
The present embodiment by embodiment 2-5 exempt from processing, non-plated film neodymium-doped rare earth orthophosphates chip is uniformly plated with 0.53,
1.06,1.34 microns of anti-reflection films improve the output power and transfer efficiency of corresponding laser to reduce cavity loss.
Claims (3)
1. a kind of preparation method for exempting to process sheet laser crystal, it is characterised in that detailed process are as follows:
(1) by Re2O3With PbHPO4It is put into platinum crucible with molar ratio 1:23 mixing, wherein Re is Nd and Y, or is Nd and Lu, neodymium
Ion doping concentration is 0.05-50at.%；PbHPO4Pb is resolved into platinum crucible2P2O7, a part of Pb2P2O7With Re2O3
Reaction generates RePO4, another part is as fluxing agent, specific chemical reaction are as follows:
Pb2P2O7+Re2O3=2RePO4+2PbO；
(2) when crystal growth, 1250 DEG C is first warming up to as early as possible from room temperature and is kept the temperature for 24 hours, start cooling growth, drop after solution-stabilized
Warm rate is 1 DEG C/h；After being down to 900 DEG C, crystal is no longer grown substantially, and the power supply for being then turned off platinum crucible makes its Temperature fall
To room temperature, is finally impregnated 2 days with the concentrated nitric acid of the mass fraction 65%-68% of boiling, crystal is separated from fluxing agent,
Obtain the surface depth of parallelism, flatness, highly polished sheet laser crystal.
2. exempting from the preparation method of processing sheet laser crystal according to claim 1, it is characterised in that the sheet laser of preparation
Crystal is the rare earth doped orthophosphates crystal of neodymium, for cubic zircon structure, molecular formula Nd:APO4, wherein A is element Y or Lu.
3. a kind of application of the sheet laser crystal using the bright preparation of claim 2 the method, it is characterised in that can be used for complete
Solid-state laser, all solid state laser put in order successively along its element of optical path direction are as follows: pumping source, laser focusing system,
End mirror, sheet laser crystal, output end mirror are pumped, wherein pumping source is semiconductor laser, and launch wavelength is directed at sheet and swashs
The laser of the absorption bands of luminescent crystal, pumping source transmitting is incident in sheet laser crystal by laser focusing system, pumps end
Be coated on mirror it is high to pump light thoroughly, to the high anti-deielectric-coating of operating laser, sheet laser crystal be it is primary, without any plus
The neodymium-doped rare earth orthophosphates crystal of work, plated film, output end mirror are coated with the deielectric-coating penetrated to operating laser part.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811038334.2A CN109097820A (en) | 2018-09-06 | 2018-09-06 | A kind of preparation method and application for exempting to process sheet laser crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811038334.2A CN109097820A (en) | 2018-09-06 | 2018-09-06 | A kind of preparation method and application for exempting to process sheet laser crystal |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103556214A (en) * | 2013-11-15 | 2014-02-05 | 青岛大学 | Method for growing rare earth lutetium phosphate laser host crystal |
| CN105603524A (en) * | 2014-11-19 | 2016-05-25 | 中国科学院新疆理化技术研究所 | Yttrium phosphate series laser crystal, preparation method and uses thereof |
-
2018
- 2018-09-06 CN CN201811038334.2A patent/CN109097820A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103556214A (en) * | 2013-11-15 | 2014-02-05 | 青岛大学 | Method for growing rare earth lutetium phosphate laser host crystal |
| CN105603524A (en) * | 2014-11-19 | 2016-05-25 | 中国科学院新疆理化技术研究所 | Yttrium phosphate series laser crystal, preparation method and uses thereof |
Non-Patent Citations (1)
| Title |
|---|
| LIANG YANG ET AL.: "Growth, spectroscopic properties, and laser action of Yb:YPO4 crystal", 《OPTICAL MATERIALS EXPRESS》 * |
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Application publication date: 20181228 |