CN113249790B - Neodymium activated ion doped Na5Lu (MoO 4) 4 crystal and preparation method and application thereof - Google Patents

Neodymium activated ion doped Na5Lu (MoO 4) 4 crystal and preparation method and application thereof Download PDF

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CN113249790B
CN113249790B CN202110578141.1A CN202110578141A CN113249790B CN 113249790 B CN113249790 B CN 113249790B CN 202110578141 A CN202110578141 A CN 202110578141A CN 113249790 B CN113249790 B CN 113249790B
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耿磊
韩硕
张守宝
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Qufu Normal University
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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
    • C30B29/32—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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
    • H01S3/16—Solid materials
    • H01S3/1601—Solid materials characterised by an active (lasing) ion
    • H01S3/1603—Solid materials characterised by an active (lasing) ion rare earth
    • H01S3/1611—Solid materials characterised by an active (lasing) ion rare earth neodymium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
    • H01S3/16—Solid materials
    • H01S3/163—Solid materials characterised by a crystal matrix
    • H01S3/1675—Solid materials characterised by a crystal matrix titanate, germanate, molybdate, tungstate

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Abstract

The invention discloses a neodymium laserActive ion doped near-infrared laser crystal lutetium sodium molybdate xNd 3+ :Na 5 Lu (1‑x) (MoO 4 ) 4 Belonging to the technical field of laser crystal. The neodymium-doped sodium lutetium molybdate xNd of the invention 3+ :Na 5 Lu (1‑x) (MoO 4 ) 4 The doping molar ratio range of the Nd is 0<x<0.3. Using 4Na 2 O–5MoO 3 Fluxing agent, solute xNd 3+ :Na 5 Lu (1‑x) (MoO 4 ) 4 Mixing with flux in the proportion of 1:1-1:4, heating and melting, and growing by top seed crystal flux method at cooling rate of 0.1-5 deg.C per day and seed crystal rod rotation speed of 10-50 rpm. xNd of the present invention 3+ :Na 5 Lu (1‑x) (MoO 4 ) 4 The single crystal can be applied to a generating medium of a laser, the laser crystal can be pumped by an LD to realize multi-wavelength continuous or pulse laser output, and the laser based on the crystal can be applied to various fields such as communication, medical treatment, industrial manufacturing, military, remote sensing and the like.

Description

Neodymium activated ion doped Na5Lu (MoO 4) 4 crystal and preparation method and application thereof
Technical Field
The invention relates to a neodymium active ion doped near-infrared laser crystal sodium lutetium molybdate xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 The preparation method, the single crystal growth and the laser generation application thereof belong to the technical field of laser crystals.
Background
LD pump Nd 3+ The ion doped crystal matrix is one of the most important ways for generating near infrared laser at present, and the all-solid-state laser (DPSSL) manufactured based on the doped crystal has the advantages of compact volume, high efficiency, high beam quality, good stability and the like, and has important application in various fields such as communication, medical treatment, industrial manufacturing and the like. Such as neodymium-doped yttrium aluminum garnet (Nd: YAG) crystals and neodymium-doped yttrium vanadate (Nd: YVO) crystals, are well developed and are commercially used. In recent years, research shows that the neodymium-doped molybdate crystal has low phonon energy, and the rare earth ion doping concentration in a molybdate system is generally high, so that the molybdate crystal has high quantum conversion efficiency, and is expected to realize continuous or ultrashort pulse output in a micro laser. In recent years, the major research on laser applications in molybdate crystals has been scheelite-type structures such as NaY (MoO) 4 ) 2 ，LiGd(MoO 4 ) 2 Etc. and has the formula ARe (MoO) 4 ) 2 (A = Li, na, K; re = Y, la, gd). And the chemical formula is A 5 Lu(MoO 4 ) 4 The scheelite-like molybdate (A = Li, na, K; re = Y, la, gd) is difficult to grow, so the fluorescent property of the scheelite-like molybdate is mainly researched for powder materials, and the research on the application of the scheelite-like molybdate as a laser crystal is less.
Disclosure of Invention
The invention provides a compound with a chemical formula of Na 5 Lu(MoO 4 ) 4 The neomolybdate laser crystal is doped with neodymium ions and grows to have a large size of xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 The single crystal is applied to a laser as a laser generating medium, multi-wavelength continuous or pulse laser output can be realized by adopting an LD pump, and the single crystal can be applied to various fields such as communication, medical treatment, industrial manufacturing, military, remote sensing and the like.
Neodymium activated ion doped Na 5 Lu(MoO 4 ) 4 A crystal of the formula xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Wherein 0 is<x<0.3, the crystal structure belongs to a tetragonal system, and the optical structure belongs to a uniaxial crystal.
The method of claim 1 in which the neodymium-activating ions are doped with Na 5 Lu(MoO 4 ) 4 The preparation method of the crystal comprises the following specific steps:
(1) Mixing Na source, lu source, mo source and Nd source in xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 The chemical dosage ratio is accurately weighed, the mixture is uniformly ground, and the xNd is obtained by high-temperature solid-phase reaction at the temperature of 550-650 DEG C 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Polycrystalline raw materials;
(2) Subjecting the xNd obtained in the step (1) to 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Mixing and grinding the polycrystalline raw material and a fluxing agent, heating to 700-900 ℃ to enable the polycrystalline raw material to be in a molten state, keeping the temperature for 10-50 hours, and slowly reducing the temperature to 1-10 ℃ above the saturation temperature; the saturation temperature is 590-680 ℃, and the saturation temperature is specifically mixed with feed liquid and cosolventThe ratio is relevant.
(3) Will contain Na 5 Lu(MoO 4 ) 4 Putting a corundum rod of the seed crystal into the molten liquid in the step (2), and starting a seed crystal rotating motor to enable the rotating speed of the seed crystal to be 10-50 rpm;
(4) Cooling at 0.1-5 deg.c/d to grow crystal to required size, and taking out the melt at constant temperature.
Wherein the Lu source is Lu 2 O 3 、LuCl 3 、Lu(NO 3 ) 3 、LuCO 3 、Lu(AC) 3 (ii) a The Nd source being Nd 2 O 3 、NdCl 3 、Nd (NO 3 ) 3 、NdCO 3 、Nd (AC) 3 (ii) a The Mo source is MoO 3 、Na 2 MoO 4 、(NH 4 ) 2 MoO 4 (ii) a The Na source is Na 2 CO 3 、Na 2 MoO 4 One or more of NaAC, naF, naCl, naOH and NaNO 3.
Wherein, the direction of the seed crystal fixed on the corundum rod in the step 3 is any direction.
Wherein, the rotation direction of the corundum rod in the step 3 can be unidirectional or bidirectional alternately, the rotation time in each direction is 2-20 minutes, and the interval in the middle is 0.5-2 minutes.
xNd made in this invention 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 The crystal mainly has three near-infrared light-emitting wave bands under the excitation of 808nm light: 890nm, 1064nm and 1339 nm, wherein 1064nm has the largest fluorescence intensity, and the fluorescence intensity is gradually increased and the fluorescence lifetime is gradually reduced from 152 mus to 126 mus as the Nd doping concentration x is increased from 0.005 to 0.1.
The invention has the beneficial effects
1. xNd of the present invention 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 The crystal can be grown by a fluxing agent method, the temperature required by the crystal growth is lower, the optical quality of the grown crystal is good, the hardness is moderate, the physical and chemical properties are stable, the crystal does not deliquesce in the air, and the crystal is convenient to use.
2. xNd of the present invention 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 The crystal can use mature LD with the wavelength of 808nm as a pumping source to generate near-infrared laser with three wavelengths of 890nm, 1064nm and 1399nm, and is applied to a solid laser as a gain medium, and the output laser can be continuously output, also can be modulated into pulse output, namely can be output by single-wavelength laser, and also can be output by multi-wavelength laser at the same time, so that the crystal can be used in a miniature all-solid laser system to generate wavelength tunable continuous laser or multi-wavelength pulse laser.
Drawings
FIG. 1 shows 0.005Nd prepared in example 1 of the present invention 3+ :Na 5 Lu 0.995 (MoO 4 ) 4 Powder X-ray diffraction pattern of the sample.
FIG. 2 shows 0.1Nd prepared in example 3 of the present invention 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Fluorescence lifetime under 808nm excitation of the sample.
FIG. 3 shows the 0.01Nd grown in example 4 of the present invention 3+ :Na 5 Lu 0.99 (MoO 4 ) 4 Ultraviolet-visible near-infrared absorption spectrogram of single crystal.
FIG. 4 shows 0.01Nd produced in example 5 of the present invention 3+ :Na 5 Lu 0.99 (MoO 4 ) 4 Laser spectrum of single crystal laser output.
FIG. 5 shows 0.01Nd produced in example 5 of the present invention 3+ :Na 5 Lu 0.99 (MoO 4 ) 4 A fluorescence spectrum output by the single crystal laser.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples, but the invention is not to be construed as being limited to the scope of the invention.
Example 1
According to the chemical formula xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Taking 0.005 as the x and weighing a certain mass of raw material Na according to the stoichiometric ratio 2 CO 3 ，Lu 2 O 3 ，MoO 3 And Nd 2 O 3 Mixing themGrinding the mixture into fine particle powder by using an agate mortar, placing the fine particle powder in a corundum crucible with the volume of 5ml, placing the corundum crucible in a muffle furnace, raising the temperature to 400 ℃ at the rate of 5 ℃ per minute, keeping the temperature for 12 hours, continuing raising the temperature to 600 ℃ at the rate of 5 ℃ per minute, keeping the temperature for reaction for 24 hours, closing a temperature controller of the muffle furnace, naturally cooling to room temperature, taking out the product, and grinding the product to obtain 0.005Nd 3+ :Na 5 Lu 0.995 (MoO 4 ) 4 Polycrystalline powder samples.
Example 2
According to the chemical formula xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Taking 0.01 as the x, and weighing a certain mass of raw material Na according to the stoichiometric ratio 2 CO 3 ，Lu 2 O 3 ，MoO 3 And Nd 2 O 3 Uniformly mixing the raw materials, grinding the mixture into fine particle powder by using an agate mortar, placing the fine particle powder in a corundum crucible with the volume of 5ml, placing the corundum crucible in a muffle furnace, raising the temperature to 500 ℃ at the rate of 5 ℃ per minute, keeping the temperature for 12 hours, continuing raising the temperature to 600 ℃ at the rate of 5 ℃ per minute, keeping the temperature for reaction for 24 hours, closing a muffle furnace temperature controller, naturally cooling to room temperature, taking out the muffle furnace temperature controller, and grinding to obtain 0.01Nd 3+ :Na 5 Lu 0.99 (MoO 4 ) 4 Polycrystalline powder samples.
Example 3
According to the chemical formula xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Taking 0.1 as the x and weighing a certain mass of raw material Na according to the stoichiometric ratio 2 CO 3 ，Lu 2 O 3 ，MoO 3 And Nd 2 O 3 Uniformly mixing the raw materials, grinding the mixture into fine particle powder by using an agate mortar, placing the fine particle powder in a corundum crucible with the volume of 5ml, placing the corundum crucible in a muffle furnace, raising the temperature to 500 ℃ at the rate of 5 ℃ per minute, keeping the temperature for 12 hours, continuing raising the temperature to 600 ℃ at the rate of 5 ℃ per minute, keeping the temperature for reaction for 24 hours, closing a muffle furnace temperature controller, naturally cooling to room temperature, taking out the muffle furnace temperature controller, and grinding to obtain 0.1Nd 3+ :Na 5 Lu 0.9 (MoO 4 ) 4 Polycrystalline powder samples.
Example 4
According to the chemical formula xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Taking 0.01 stoichiometric ratio as the x, weighing 100g of raw material Na 2 CO 3 ，Lu 2 O 3 ，MoO 3 And Nd 2 O 3 And fluxing agent 4Na 2 O–5MoO 3 Weighing Na according to the material amount of 1:2 2 CO 3 And MoO 3 Grinding the raw materials in a mixing bowl, placing the ground raw materials in a platinum crucible, heating to 850 ℃, keeping the temperature for 50 hours to ensure that a sample fully reacts, measuring the saturation temperature to be 650 ℃, introducing seed crystals, rotating the seed crystals at the speed of 15 revolutions per minute at the cooling speed of 1 ℃ per day, and extracting the liquid level when the crystals grow to the proper size to obtain centimeter-grade 0.01Nd 3+ :Na 5 Lu 0.99 (MoO 4 ) 4 。
Example 5
0.01Nd was grown in example 4 3+ :Na 5 Lu 0.99 (MoO 4 ) 4 The laser crystal is used as a working medium of an all-solid-state laser, can generate wavelength-tunable continuous laser or multi-wavelength pulse laser, and can be widely applied to the fields of communication, medical treatment, manufacturing, military, remote sensing and the like.
The technical solutions and specific embodiments disclosed above are only for further description of the present invention, and should not be taken as limitations to the content of the present invention, and the accompanying drawings should also be understood as one of the embodiments of the present invention, and those skilled in the art should also make additions, modifications, similar substitutions and the like without creatively making the base of the present invention without departing from the spirit of the present invention, and shall be within the protection scope of the present invention.

Claims (7)

1. Neodymium-activated ion doped Na 5 Lu(MoO 4 ) 4 A crystal characterized by the formula xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Wherein x is 0.005 to 0.1, the matrix structure belongs to a tetragonal system, and the space group I4 1 /a Z, unit cell parameters a = b =11.323 Å, c = 11.385 Å;
the neodymium active ions are doped with Na 5 Lu(MoO 4 ) 4 The preparation method of the crystal comprises the following steps:
(1) Mixing Na source, lu source, mo source and Nd source in xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 The chemical dosage ratio is accurately weighed, then the mixture is evenly ground, and the xNd is obtained by high-temperature solid phase reaction at the temperature of 550-650 DEG C 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Polycrystalline raw materials;
(2) Subjecting the xNd obtained in step (1) to 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Polycrystalline raw material and flux 4Na 2 O–5MoO 3 Mixing, grinding, heating to 700-900 deg.C to melt, holding at constant temperature for 10-50 hr, and slowly cooling to 1-10 deg.C above saturation temperature;
(3) Will contain Na 5 Lu(MoO 4 ) 4 Putting a corundum rod of the seed crystal into the molten liquid in the step (2), and starting a seed crystal rotating motor to enable the rotating speed of the seed crystal to be 10-50 rpm;
(4) Cooling at 0.1-5 deg.c/d to grow crystal to required size, and taking out the melt at constant temperature.
2. The neodymium-activated ion doped Na of claim 1 5 Lu(MoO 4 ) 4 The preparation method of the crystal is characterized by comprising the following specific steps:
(1) Mixing Na source, lu source, mo source and Nd source in xNd 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 The chemical dosage ratio is accurately weighed, the mixture is uniformly ground, and the xNd is obtained by high-temperature solid-phase reaction at the temperature of 550-650 DEG C 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Polycrystalline raw materials;
(2) Subjecting the xNd obtained in the step (1) to 3+ :Na 5 Lu (1-x) (MoO 4 ) 4 Polycrystalline raw material and flux 4Na 2 O–5MoO 3 Mixing, grinding, heating to 700-900 deg.C to melt, holding at constant temperature for 10-50 hr, and slowly cooling to 1-10 deg.C above saturation temperature;
(3) Will contain Na 5 Lu(MoO 4 ) 4 Putting a corundum rod of the seed crystal into the molten liquid in the step (2), and starting a seed crystal rotating motor to enable the rotating speed of the seed crystal to be 10-50 rpm;
(4) Cooling at 0.1-5 deg.c/d to grow crystal to required size, and taking out the melt at constant temperature.
3. The method of claim 2, wherein the Lu source is Lu 2 O 3 、LuCl 3 、Lu(NO 3 ) 3 、LuCO 3 、Lu(AC) 3 One of (1); the Nd source being Nd 2 O 3 、NdCl 3 、Nd (NO 3 ) 3 、NdCO 3 、Nd (AC) 3 One of (a) and (b); mo source is MoO 3 、Na 2 MoO 4 、(NH 4 ) 2 MoO 4 One of (1); the Na source is Na 2 CO 3 、Na 2 MoO 4 、NaAC、NaF、NaCl、NaOH、NaNO 3 One kind of (1).
4. A production method according to claim 2, wherein the direction of the seed crystal fixed to the corundum rod in step 3 is arbitrary.
5. The method according to claim 2, wherein the rotation direction of the corundum rod in step 3 can be unidirectional or bidirectional, and the rotation time in each direction is 2-20 minutes, and the interval between the rotation directions is 0.5-2 minutes.
6. The neodymium-activated ion doped Na of claim 1 5 Lu(MoO 4 ) 4 Use of a crystal for the production of a single-wavelength or multi-wavelength, continuous or pulsed laser light of around 1 μm.
7. The use according to claim 6, characterized by continuous or pulsed emission of multiwavelength laser in the 1059-1065nm band when pumped with a laser diode with a wavelength of 586nm or 808 nm.
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