CN108330541A - A kind of GYAP laser crystals and preparation method thereof - Google Patents
A kind of GYAP laser crystals and preparation method thereof Download PDFInfo
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- CN108330541A CN108330541A CN201810052676.3A CN201810052676A CN108330541A CN 108330541 A CN108330541 A CN 108330541A CN 201810052676 A CN201810052676 A CN 201810052676A CN 108330541 A CN108330541 A CN 108330541A
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- gyap
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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
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/24—Complex oxides with formula AMeO3, wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. ortho ferrites
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
Abstract
The invention discloses a kind of GYAP laser crystal materials and preparation method thereof, are related to a kind of laser crystal host material, the chemical formula of the crystalline material is GdxY1‑xAlO3, wherein 0.01≤x≤0.99, which belongs to orthorhombic system perovskite structure, Gd3+And Y3+It is randomly dispersed in and is located at AlO6On case between octahedral layer, which has disordered structure, and Gd is prepared for using Czochralski method3+And Y3+The GYAP crystal of different proportion, grows transparent, and integrality is good, the GYAP crystal of good in optical property.Use the crystal as host doped active ions, Absorption and fluorescence spectrum has wider full width at half maximum (FWHM), there is important application in social production, military affairs, medicine, scientific domain.
Description
Technical field
The present invention relates to laser material preparing technical fields, and in particular to a kind of GYAP laser crystals and preparation method thereof.
Background technology
In recent years, it with the fast development of laser technology, is obtained extensively in numerous areas such as optics, communication, medicine, military affairs
Using having that small, price is low, all solid state laser of advantages of simple structure and simple receives the concern of people.All-solid state laser
It is exactly by host crystal and active ions group that laser crystal material in device has direct influence, laser crystal to the laser of generation
At shining for active ions has close relationship, the absorption of rear-earth-doped light emitting ionic with the matrix cation case substituted
The symmetry of case is related residing for depending on rare earth ion with fluorescence spectrum.Symmetry is lower, and the uneven broadening of spectrum is brighter
It is aobvious.
GYAP (aluminic acid gadolinium yttrium) is a kind of novel laser crystal host material of function admirable, molecule GdYAlO3, belong to
Orthorhombic system perovskite structure, due to Gd3+And Y3+Ionic radius be closer to, therefore mix a certain number of Gd3+Instead of Y3+
Case in crystal is will not to cause the larger distortion of lattice, and Gd3+And Y3+It is randomly dispersed in and is located at AlO6Octahedral layer it
Between case, cause the case of crystal substrate interior section ion to be not fixed in this way, have certain degree of disorder, the unordered journey of crystal
Degree is higher, can lead to the non-uniform broadening of Absorption and fluorescence spectrum, and then is crystalline host material as working media
The solid state laser pumped in LD is applied to bring significant advantage.For GYAP crystal, Gd3+And Y3+Ratio it is different,
The internal structure of matrix opposite can also change, also just different to the broadening of Absorption and fluorescence spectrum.
Invention content
The purpose of the present invention is to solve drawbacks described above in the prior art, a kind of GYAP laser crystals and its system are provided
Preparation Method.
According to disclosed embodiment, the first aspect of the present invention discloses a kind of GYAP laser crystals, and the GYAP swashs
Luminescent crystal is using GYAP as laser crystal host material, Gd3+Ion and Y3+Ion is randomly dispersed in positioned at AlO6Octahedral layer it
Between case on, have highly disordered lattice structure,
The chemical formula of the GYAP laser crystals is：GdxY1-xAlO3, wherein 0.01≤x≤0.99, and meet
Chemical equation：
x Gd2O3+(1-x)Y2O3+Al2O3=2GdxY1-xAlO3。
Further, the Gd3+Ion and the Y3+Ion optimization ion as other side simultaneously, increase lattice
The degree of disorder.
According to disclosed embodiment, the second aspect of the present invention discloses a kind of preparation method of GYAP laser crystals, institute
The preparation method stated includes the following steps：
S1, according to chemical formula GdxY1-xAlO3Mole atom than weigh Gd2O3、Y2O3And Al2O3As raw material, raw material warp
It grinds and is mixed even rear briquetting sintering；
S2, the raw material sintered is fitted into iridium crucible, is replaced in single crystal growing furnace completely with high pure nitrogen or inert gas
Air, crystal oven is warming up to 1850~1950 DEG C, and crystal pull speed is 0.6~1.5mm/h, and rotating speed is 8~20rpm；
S3, when temperature is increased to 1850~1950 DEG C, carry out it is roasting brilliant, sow, necking down, shouldering, the isometrical stage, in crystal
After growth reaches predetermined size, finishing phase is carried out；
S4, crystal is pulled away from 0.2~1.5cm of melt, is then slowly dropped to room temperature, grows GYAP monocrystalline, wherein drop
Temperature is divided into 4 stages：
Constant temperature 2~10h, 1850 DEG C~1950 DEG C；
15~25 DEG C/h, cools down and continue 10~20h, 1850 DEG C~1700 DEG C；
25~35 DEG C/h, cools down and continue 20~30h, 1700 DEG C~1200 DEG C；
40~45 DEG C/h, cools down and continue 30~40h, 1200 DEG C~1300 DEG C to room temperature.
Further, crystal growth rate is controlled by the way of gradual change in necking down in the step S3, avoid big
Amplitude adjusted power.
Further, it needs slowly to cool down near growth temperature in the step S4, falling temperature gradient 15~40
℃/h。
Further, the step S1 is specially：
Using Medium frequency induction Czochralski grown GYAP crystal, heater is iridium crucible, according to chemical formula GdxY1-xAlO3Rub
You weigh Gd by atomic ratio2O3、Y2O3And Al2O3As raw material, raw material through grind be mixed it is even after, compressed under hydraulic press and blocking pass through height
Warm solid-phase synthesis, temperature are 1000~1200 DEG C, and sintering time 20~30 hours is down to room temperature, at obtaining GYAP after conjunction
Polycrystalline fluorescent material.
Further, the step S2 further includes：
It is put into seed rod using the GYAP seed crystals of a axis or b axis, is packed into burner hearth together.
The present invention has the following advantages and effects with respect to the prior art：
1) crystal belongs to orthorhombic system perovskite structure, Gd3+And Y3+It is randomly dispersed in and is located at AlO6Between octahedral layer
Case on, the crystal have disordered structure, Gd is prepared for using Czochralski method3+And Y3+The GYAP crystal of different proportion, it is raw
Grow transparent, integrality is good, the GYAP crystal of good in optical property.
2) crystal has wider full width at half maximum (FWHM) as host doped active ions, Absorption and fluorescence spectrum,
There is important application in social production, military affairs, medicine, scientific domain.
Description of the drawings
Fig. 1 is a kind of process step figure of GYAP laser crystals preparation method disclosed by the invention.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
The every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Embodiment one
Present embodiment discloses a kind of using GYAP as the laser crystal host material of matrix, and GYAP crystal is since it is with nothing
Sequence structure can increase the uneven broadening of the active ions Absorption and fluorescence spectrum of doping, in communication, medical treatment, scientific research
And there is important application prospect in the fields such as military affairs.
It is a kind of using GYAP as the laser crystal host material of matrix, chemical formula is：GdxY1-xAlO3, wherein 0.01≤x≤
0.99, which meets chemical equation：
x Gd2O3+(1-x)Y2O3+Al2O3=2GdxY1-xAlO3；
Gd3+And Y3+It is randomly dispersed in and is located at AlO6On case between octahedral layer, there is highly disordered lattice structure.
Gd3+Ion, Y3+Ion can increase the degree of disorder of lattice simultaneously as the optimization ion of other side.
The crystal can realize wide band absorption spectrum and fluorescence spectrum, and the Solid State Laser made of the crystal can be realized super
Short laser pulse exports, and is widely used in the fields such as social production, military affairs, medicine, science.
Embodiment two
Present embodiment discloses a kind of using GYAP as the laser crystal preparation method of matrix, specifically includes following steps：
Using Medium frequency induction Czochralski grown GYAP crystal, heater is iridium crucible, according to chemical formula GdxY1-xAlO3Rub
You weigh Gd by atomic ratio2O3(99.999%), Y2O3(99.999%) and Al2O3(99.999%) it is used as raw material, raw material mixed through grinding
After uniformly, compressed under hydraulic press blocking by high temperature solid phase synthesis, temperature is 1000~1200 DEG C, sintering time 20~
30 hours, it is down to room temperature, at obtaining GYAP polycrystalline fluorescent materials after conjunction.The raw material sintered is put into iridium crucible, is used
Be that the GYAP seed crystals of a axis or b axis are put into seed rod, be packed into burner hearth together.
By monocrystalline stove evacuation, be passed through nitrogen prevents iridium crucible high temperature from being aoxidized as protective gas, and growth temperature is
1850~1950 DEG C, pull rate is 0.6~1.5mm/h, and crystal rotation is 8~20rpm, and thermal insulation material is using oxidation
Zirconium, and use sapphire and corundum piece to build better heat-insulation system, sapphire is placed on the watch window of insulation cover, due to indigo plant
Jewel piece polishing both surfaces, transparency is high, the growing state of crystal can be observed by sapphire sheet, corundum piece is placed on insulation cover top
Portion, to provide the thermal field of suitable crystal growth.
When temperature is increased to 1850~1950 DEG C, roasting crystalline substance is carried out, is sowed, necking down, shouldering is isometrical to wait the stages, in necking down
When need to control crystal growth rate, avoid significantly regulation power, controlled by the way of gradual change.Reach predetermined in crystal growth
After size, finishing phase is carried out, herein it should be noted that crystal is pulled away from 0.2~1.5cm of melt, does not answer excessively high cause because of temperature
Crystal cleavage caused by variation is big.
Crystal needs to set cooling process after being pulled away from melt, is slowly dropped to room temperature, and cooling is divided into 4 stages：
1. constant temperature 2~10h, 1850~1950 DEG C；
2. 15~25 DEG C/h, cools down and continue 10~20h, 1850 DEG C~1700 DEG C；
3. 25~35 DEG C/h, cools down and continue 20~30h, 1700 DEG C~1200 DEG C；
4. 40~45 DEG C/h, cools down and continue 30~40h, 1200 DEG C~1300 DEG C to room temperature；
Crystal needs slowly to cool down near growth temperature, prevents from making crystal cleavage because temperature change is excessive,
Slow cooling is also the temperature gradient for reducing crystal growth, the phenomenon that overcoming crystal cleavage, is finally grown by cooling
GYAP monocrystalline, crystal pale yellow transparent, does not crack, and optical property is preferable.
Embodiment three
Using Medium frequency induction Czochralski grown GYAP crystal, raw material Gd2O3(99.999%), Y2O3(99.999%) and
Al2O3(99.999%), it is sintered by high temperature solid-state method, is put into burned raw material and existsIridium crucible in, furnace body
High pure nitrogen is filled with after vacuumizing as protective gas, growth temperature is 1850 DEG C, pull rate 1.4mm/h, crystal rotation
For 10rpm, manual Rapid lifting is carried out when crystal equal-diameter part reaches 50mm makes it be detached from melt, and sets cooling journey
Sequence obtains the G of a 28 × 65mm of a axis φ0.1Y0.9AP crystal, crystal pale yellow transparent, integrality is good, and optical property is preferable.
Example IV
The raw material Y for selecting purity to be more than 99.999% in the present embodiment2O3、Al2O3、Gd2O3, carried out using czochralski method
G0.9Y0.1AP crystal growths, raw material are sintered by high temperature solid-state method, are put into crucible and heat, about 1900 DEG C of growth temperature, lifting
Speed is 1.1mm/h, crystal rotation 10rpm, the insulation cover with watch window of use, and sapphire sheet is placed on heat insulation window
Mouthful, to provide crystal growth suitable thermal field, manual Rapid lifting is carried out when crystal equal-diameter part reaches 50mm to be made it and melts
Body is detached from, and sets cooling process, obtains the G of a 28 × 62mm of a axis φ0.9Y0.1AP crystal, crystal pale yellow transparent are complete
Whole property is good, and optical property is preferable.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (7)
1. a kind of GYAP laser crystals, which is characterized in that the GYAP laser crystals are using GYAP as laser crystal matrix material
Material, Gd3+Ion and Y3+Ion is randomly dispersed in positioned at AlO6On case between octahedral layer, there is highly disordered lattice knot
Structure,
The chemical formula of the GYAP laser crystals is：GdxY1-xAlO3, wherein 0.01≤x≤0.99, and meet chemical
Equation：
x Gd2O3+(1-x)Y2O3+Al2O3=2GdxY1-xAlO3。
2. a kind of GYAP laser crystals according to claim 1, which is characterized in that the Gd3+Ion and the Y3+
Ion optimization ion as other side simultaneously, increases the degree of disorder of lattice.
3. a kind of preparation method of GYAP laser crystals, which is characterized in that the preparation method includes the following steps：
S1, according to chemical formula GdxY1-xAlO3Mole atom than weigh Gd2O3、Y2O3And Al2O3As raw material, raw material is mixed through grinding
Briquetting sintering after uniformly；
S2, the raw material sintered is fitted into iridium crucible, replaces the sky in single crystal growing furnace completely with high pure nitrogen or inert gas
Gas, crystal oven are warming up to 1850~1950 DEG C, and crystal pull speed is 0.6~1.5mm/h, and rotating speed is 8~20rpm；
S3, when temperature is increased to 1850~1950 DEG C, carry out it is roasting brilliant, sow, necking down, shouldering, the isometrical stage, in crystal growth
After reaching predetermined size, finishing phase is carried out；
S4, crystal is pulled away from 0.2~1.5cm of melt, is then slowly dropped to room temperature, grows GYAP monocrystalline, wherein cooling point
For 4 stages：
Constant temperature 2~10h, 1850~1950 DEG C；
15~25 DEG C/h, cools down and continue 10~20h, 1850 DEG C~1700 DEG C；
25~35 DEG C/h, cools down and continue 20~30h, 1700 DEG C~1200 DEG C；
40~45 DEG C/h, cools down and continue 30~40h, 1200 DEG C~1300 DEG C to room temperature.
4. a kind of preparation method of GYAP laser crystals according to claim 3, which is characterized in that in the step S3
Crystal growth rate is controlled by the way of gradual change in necking down, avoids significantly regulation power.
5. a kind of preparation method of GYAP laser crystals according to claim 3, which is characterized in that in the step S4
It needs slowly to cool down near growth temperature, 15~40 DEG C/h of falling temperature gradient.
6. a kind of preparation method of GYAP laser crystals according to claim 3, which is characterized in that the step S1 tools
Body is：
Using Medium frequency induction Czochralski grown GYAP crystal, heater is iridium crucible, according to chemical formula GdxY1-xAlO3Mole original
Son is than weighing Gd2O3、Y2O3And Al2O3As raw material, raw material through grind be mixed it is even after, compressed under hydraulic press blocking solid by high temperature
Phase synthesi, temperature are 1000~1200 DEG C, and sintering time 20~30 hours is down to room temperature, at obtaining GYAP polycrystalline after conjunction
Fluorescent material.
7. a kind of preparation method of GYAP laser crystals according to claim 3, which is characterized in that the step S2 is also
Including：
It is put into seed rod using the GYAP seed crystals of a axis or b axis, is packed into burner hearth together.
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| CN112952544A (en) * | 2021-01-18 | 2021-06-11 | 枣庄学院 | Dysprosium terbium aluminum tri-doped yellow laser crystal and preparation method and application thereof |
| CN112941630A (en) * | 2021-01-18 | 2021-06-11 | 枣庄学院 | Dysprosium, lutecium and aluminum triple-doped lanthanum calcium gallate intermediate infrared laser crystal and preparation method and application thereof |
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Application publication date: 20180727 |