CN112359419A - Czochralski method for growing rare earth ion doped silicate eutectic material and preparation method thereof - Google Patents

Czochralski method for growing rare earth ion doped silicate eutectic material and preparation method thereof Download PDF

Info

Publication number
CN112359419A
CN112359419A CN202011147283.4A CN202011147283A CN112359419A CN 112359419 A CN112359419 A CN 112359419A CN 202011147283 A CN202011147283 A CN 202011147283A CN 112359419 A CN112359419 A CN 112359419A
Authority
CN
China
Prior art keywords
rare earth
earth ion
ions
molar ratio
raw material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011147283.4A
Other languages
Chinese (zh)
Inventor
李纳
徐军
徐晓东
王东海
王庆国
唐慧丽
吴锋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing Tongli Crystal Material Research Institute Co ltd
Original Assignee
Nanjing Tongli Crystal Material Research Institute Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing Tongli Crystal Material Research Institute Co ltd filed Critical Nanjing Tongli Crystal Material Research Institute Co ltd
Priority to CN202011147283.4A priority Critical patent/CN112359419A/en
Publication of CN112359419A publication Critical patent/CN112359419A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention provides a Czochralski method for growing rare earth ion doped silicate eutectic material with a chemical formula of Re4xBi4(1‑x)Si3O12/Bi12SiO20Wherein, the rare earth ion Re is any one of Nd, Yb, Tm, Ho, Er, Pr, Dy and Sm, the value range of X is 0.003-0.05, and simultaneously, the preparation method of the eutectic material is also provided, and Bi with certain quality purity of 5N is adopted2O3、SiO2And Re2O3The raw materials are fully ground, pressed into blocks, sintered at high temperature and grown by a Czochralski method to obtain the eutectic crystal. Compared with the prior art, the eutectic material can have crystal grains with two sizes in the material, and the luminous full width at half maximum of rare earth ions is wider than that in a single crystal material, so that the eutectic material can be used for tunable laser output.

Description

Czochralski method for growing rare earth ion doped silicate eutectic material and preparation method thereof
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a rare earth ion doped silicate eutectic material grown by a pulling method and a preparation method thereof.
Background
With the development of the information age, people pay more and more attention to the special-band laser, and the research center of gravity of worldwide scholars is promoted to be changed to the direction of a new-band excellent laser, such as a visible light band and a middle infrared band with longer wavelength. GaN blue diodes today already can provide output power in the order of watts near the 390nm band. InGaN diodes may lase from near-uv to blue in the 360-470nm wavelength range.
Trivalent Pr3+More doping ions which directly emit visible light laser are applied. At 445nm, 468nm and 486nm, Pr3+Can reach 10-19cm2Magnitude, upper energy level thereof3P0The fluorescence lifetime of (a) is about several tens of microseconds. Wherein, the absorption peak at 445nm is very consistent with the emission wavelength of the InGaN laser diode pumping source, and the absorption peak at 468nm is very consistent with the emission wavelength of the 2 omega-OPSLs pumping source. Pr compared to other rare earth ions3+In the visible light wave band range, the LED lamp has a large number of radiation transitions, and the light emitting range of the LED lamp almost covers red light, orange light, green light and blue light of the visible light wave band. Thus Pr3+Doped laser materials are currently the most promising visible band laser materials. Yet Pr3+One problem that is faced is that there is no corresponding energy level transition in the yellow band alone. The yellow laser has great application value, for example, 589nm yellow light can be used in the fields of sodium beacon lasers, scientific research, remote sensing and the like. Dy (Dy)3+Comprising seven 4f-4f level transitions, of which the intensity is highest4F9/2→6H13/2The transition is just in the yellow light emission band, so in the research of yellow band laser, Dy3+Many significant advances have also been made. And Dy3+The effects of (1) are similar3+Is rare earth ion except Dy3+The only other one is the ion present for a yellow energy level transition. In addition, Yb3+、Nd3+、Tm3+、Ho3+、Er3+Laser output has been obtained with doped hosts (glass, ceramic and crystal).
However, rare earth ion doped silicate (BSO) eutectic materials have not been reported. The eutectic crystal has two crystal phases in the crystal structure, so that the emission bandwidth of rare earth ions can be improved to further obtain Q-switched laser output. Therefore, it is necessary to research a rare earth ion-doped eutectic laser material having a eutectic structure.
Disclosure of Invention
In order to solve the defects of the prior art, the invention improves and obtains the eutectic material consisting of crystal grains with two sizes in the material, and particularly provides a Czochralski-method-grown rare earth ion-doped silicate eutectic material with the chemical formula of Re4xBi4(1-x)Si3O12/Bi12SiO20Wherein, the rare earth ion Re is any one of Nd, Yb, Tm, Ho, Er, Pr, Dy and Sm, and the value range of x is 0.003-0.05.
As an improvement, the raw material adopted is Bi with the purity of 5N2O3、SiO2And Re2O3In which Bi2O3And SiO2The mass fraction ratio of (1): 3.
as an improvement, in the raw materials (when the rare earth ion Re is Nd, the molar ratio of Nd to Bi ions is 0.003-0.1:1, when the rare earth ion Re is Yb, the molar ratio of Yb to Bi ions is 0.5-1:1, when the rare earth ion Re is Tm, the molar ratio of Tm to Bi ions is 0.02:0.98, when the rare earth ion Re is Ho, the molar ratio of Ho to Bi ions is 0.003-0.005: 0.995-0.997, when the rare earth ion Re is Er, the molar ratio of Er to Bi ions is 0.03-0.07: 0.97-0.93, when the rare earth ion Re is Pr, the molar ratio of Pr to Bi ions is 0.003-0.990.994: 0.006: 0.97, when the rare earth ion Re is Sm 0.05-0.05: 0.05 to 98, as a specific implementation manner of the invention, the invention also provides a preparation method of the rare earth ion doped silicate eutectic material grown by the pulling method, the eutectic material is any one of the eutectic materials, and the specific steps are as follows:
s01, weighing the powder raw materials;
according to the mole percentage of 1: 3 weighing Bi with the purity of 5N2O3、SiO2The powder is doped with a certain amount of rare earth oxide, wherein the molar ratio of rare earth ions Re to Bi ions in the rare earth oxide is Re: and Bi is X: 1-X, wherein the value of X is 0.003-0.05, weighing, the raw material is 200-350g, and putting the raw material into an agate mortar for fully grinding to uniformly mix the raw material;
s02, pressing the blank and sintering at high temperature
Pressing the ground raw material S01 by adopting a hydraulic press, pressing the raw material into a block blank, and sintering at 480-650 ℃ for 8-17h for forming to obtain a polycrystalline raw material;
s03, charging
Placing the seed crystal, the crucible center and the coil center on the same vertical line, then placing the seed crystal, the crucible center and the coil center into a pulling furnace for growth, starting a mechanical pump for vacuum pumping, filling inert gas as protective atmosphere, and completing furnace charging;
s04, growing
Heating up, heating up within 1.5-2.8h and keeping constant temperature to ensure that the raw materials in the crucible are completely melted, wherein the growth process comprises seeding, shouldering and diameter equalization, slowly cooling to room temperature after the growth is finished, and taking out the crystal. As a modification, the grinding time of the powder raw material in the step S01 is 40-60 min.
As an improvement, in the step S02, the pressing pressure of the hydraulic press is 15-35MPa, and the pressing time is 5-10 min.
As an improvement, after the growth is finished in the step S04, the temperature reduction time is 10-15h, so that the crystal cracking caused by the excessively high temperature reduction rate is prevented.
As a modification, in step S01, the rare earth ion Re in the raw material is any one of Nd, Yb, Tm, Ho, Er, Pr, Dy, and Sm, and when the rare earth ion Re is any one of the above, the molar ratios of the rare earth ion Re to the Bi ion are, independently: nd, Bi is 0.003-0.1: 1; 0.5-1:1 of Yb and Bi; tm is 0.02: 0.98; and Ho, Bi is 0.003-0.005: 0.995-0.997; er, Bi is 0.03-0.07: 0.97-0.93; bi is 0.003-0.006: 0.994-0.997; bi is 0.02-0.04: 0.96-0.98; 0.03-0.05% of Sm and Bi: 10.957-0.975. .
Has the advantages that: compared with the prior art, the Re provided by the invention4xBi4(1-x)Si3O12/Bi12SiO20The eutectic material can obtain crystal grains with two sizes in the material, wherein the rare earth ion Re is any one of Nd, Yb, Tm, Ho, Er, Pr, Dy and Sm, and has wider luminescence full width at half maximum ratio in the single crystal material, and the material has greater advantages compared with the existing material for tunable laser output.
Detailed Description
The present invention is further illustrated below with reference to examples.
A rare earth ion doped silicate eutectic material grown by a pulling method has a chemical formula of Re4xBi4(1-x)Si3O12/Bi12SiO20Wherein, the rare earth ion Re is any one of Nd, Yb, Tm, Ho, Er, Pr, Dy and Sm, and the value range of x is 0.003-0.05. The raw material is Bi with the purity of 5N2O3、SiO2And Re2O3In which Bi2O3And SiO2The mass fraction ratio of (1): 3.
as a specific embodiment of the present invention, when the rare earth ion Re in the raw material is Nd, the molar ratio of Nd to Bi ions is: nd: 0.003-0.1 of Bi: 1; when the rare earth ion Re is Yb, the molar ratio of Yb to Bi ions is Yb: 0.5-1 of Bi: 1; when the rare earth ion Re is Tm, the molar ratio Tm of Tm to Bi ions is as follows: and Bi is 0.02:0.98 of; when the rare earth ion Re is Ho, the molar ratio Ho of Ho to Bi ions: 0.003-0.005% of Bi: 0.995-0.997; when the rare earth ion Re is Er, the molar ratio of Er to Bi ions is Er: 0.03-0.07% of Bi: 0.97-0.93; when the rare earth ion Re is Pr, the molar ratio Pr of Pr to Bi ions is as follows: bi is 0.003-0.006: 0.994-0.997; when the rare earth ion Re is Dy, the molar ratio of Dy to Bi ions is 0.02-0.04: 0.96-0.98; when the rare earth ion Re is Sm, the molar ratio of Sm to Bi ions is Sm: 0.03-0.05% of Bi: 0.95-0.97. In order to prepare the eutectic material, the method adopted by the invention comprises the following specific steps:
s01, weighing the powder raw materials;
according to the mole percentage of 1: 3 weighing Bi with the purity of 5N2O3、SiO2The powder is doped with a certain amount of rare earth oxide, wherein the molar ratio of rare earth ions Re to Bi ions in the rare earth oxide is Re: and Bi is X: 1-X, wherein the value of X is 0.003-0.05, weighing, the raw material is 200-350g, and putting the raw material into an agate mortar for fully grinding to uniformly mix the raw material; in the step S01, the grinding time of the powder raw material is 40-60 min.
S02, pressing the blank and sintering at high temperature
Pressing the ground raw material S01 by adopting a hydraulic press, pressing the raw material into a block blank, and sintering at 480-650 ℃ for 8-17h for forming to obtain a polycrystalline raw material; in the step S02, the pressing pressure of the hydraulic press is 15-35MPa, and the pressing time is 5-10 min.
S03, charging
Placing the seed crystal, the crucible center and the coil center on the same vertical line, then placing the seed crystal, the crucible center and the coil center into a pulling furnace for growth, starting a mechanical pump for vacuum pumping, filling inert gas as protective atmosphere, and completing furnace charging;
s04, growing
Heating up, heating up within 1.5-2.8h and keeping constant temperature to ensure that the raw materials in the crucible are completely melted, wherein the growth process comprises seeding, shouldering and diameter equalization, slowly cooling to room temperature after the growth is finished, and taking out the crystal. And after the growth in the step S04 is finished, the cooling time is 10-15h, so that the crystal cracking caused by the excessively high cooling rate is prevented.
As a specific embodiment of the present invention, in the raw material in step S01, the rare earth ion Re is any one of Nd, Yb, Tm, Ho, Er, Pr, Dy, and Sm, and when the rare earth ion Re is any one of the above, the molar ratio of the rare earth ion Re to the Bi ion is, independently: nd, Bi is 0.003-0.1: 1; 0.5-1:1 of Yb and Bi; tm is 0.02: 0.98; and Ho, Bi is 0.003-0.005: 0.995-0.997; er, Bi is 0.03-0.07: 10.97-0.93; bi is 0.003-0.006: 0.994-0.997; bi is 0.02-0.043: 10.96-0.987; 0.03-0.05% of Sm and Bi: 0.95-0.97. In order to better illustrate the eutectic material of the present invention, the following examples are given in detail.
Example 1
A Czochralski method for growing a rare earth ion doped silicate eutectic material comprises the following steps:
(1) weighing the powder raw materials; according to Bi2O3-SiO2Binary phase diagram, Bi2O3Is 25% of SiO2Is 75 mol percent, is doped with rare earth ion Nd3+And Bi3+The molar ratio of ions is Nd: and Bi is 0.003: 1. Bi with the purity of 5N2O3、SiO2And Nd2O3The powders were weighed according to the above molar ratio, the total raw materials was 300g, and sufficiently ground for 40min to mix the raw materials uniformly.
(2) Pressing the ground raw materials into blocks by adopting a hydraulic press, wherein the pressure of the hydraulic press is 15MPa, the pressing time is 10min, and the blocks are formed by high-temperature sintering at 480 ℃ for 17h to form a polycrystalline raw material;
(3) putting a polycrystalline raw material into a microporous crucible, and putting rare earth ion doped silicate, namely BSO seed crystal into a seed crystal groove and fixing the BSO seed crystal by using screws;
(4) after the charging is finished, the temperature is raised, and whether the molten material flows out from the crucible opening or not is observed to further adjust the power so as to ensure that the raw materials in the crucible are completely melted.
(5) Slowly increasing the pulling speed to crystallize the molten material, and keeping the pulling speed constant after the growth is stable. After all the raw materials in the crucible are pulled out, the temperature is reduced for 10 hours, after the temperature is reduced to room temperature, the crystal growth is finished, if the temperature reduction time is short, the crystal is cracked, and the quality is poor.
Compared with the existing single crystal material, the crystal generated by the method has a luminous half-height-width ratio value of the tested rare earth ions which is wider than that of the single crystal material, and can be used for tunable laser output.
Example 2
A Czochralski method for growing a rare earth ion doped silicate eutectic material comprises the following steps:
(1) weighing the powder raw materials; according to Bi2O3-SiO2Binary phase diagram, Bi2O3Is 25% of SiO2Is 75 mol percent, is doped with rare earth ion Yb3+And Bi3+The ion molar ratio is Yb: bi of 5N purity is added to the mixture in a ratio of 0.005:12O3、SiO2And Yb2O3The powders are weighed according to the above molar ratio, the total weight of the raw materials is 300g, and the raw materials are fully ground for 60min to be uniformly mixed.
(2) Pressing the ground raw materials into blocks by adopting a hydraulic press, wherein the pressure of the hydraulic press is 35MPa, the pressing time is 5min, and the blocks are sintered at the high temperature of 600 ℃ for 8h to form a polycrystalline raw material;
(3) putting a polycrystalline raw material into a microporous crucible, and putting rare earth ion doped silicate, namely BSO seed crystal into a seed crystal groove and fixing the BSO seed crystal by using screws;
(4) after charging, heating is carried out, and whether the crucible opening has melt flowing out and the power is adjusted is observed, so that the raw materials in the crucible are completely melted.
(5) Slowly increasing the pulling speed to crystallize the molten material, and keeping the pulling speed constant after the growth is stable. After all the raw materials in the crucible are pulled out, the temperature is reduced for 15h, after the temperature is reduced to room temperature, the crystal growth is finished, and if the temperature reduction time is short, the crystal will crack, and the quality is poor.
Compared with the existing single crystal material, the crystal generated by the method has wider luminous half-height-width ratio of the rare earth ions in the single crystal material through testing, and can be used for tunable laser output.
Example 3
A Czochralski method for growing a rare earth ion doped silicate eutectic material comprises the following steps:
(1) weighing the powder raw materials; according to Bi2O3-SiO2Binary phase diagram, Bi2O3Is 25% of SiO2Is 75 percent by mol, is doped with rare earth ion Pr3+And Bi3+The molar ratio of ions is Pr: and Bi is 0.006: 0.994. Bi with the purity of 5N2O3、SiO2And Pr6O11The powders were weighed in the above molar ratio, 300g in total, and sufficiently ground for 55min to mix the raw materials uniformly.
(2) Pressing the ground raw materials into blocks by adopting a hydraulic press, wherein the pressure of the hydraulic press is 20MPa, the pressing time is 8min, and the blocks are sintered at the high temperature of 520 ℃ for 13h to form polycrystalline raw materials;
(3) putting a polycrystalline raw material into a crucible, and putting rare earth ion doped silicate, namely BSO seed crystal into a seed crystal groove and fixing the BSO seed crystal by using screws;
(4) after charging, heating is carried out, and whether the crucible opening has melt flowing out and the power is adjusted is observed, so that the raw materials in the crucible are completely melted.
(5) Slowly increasing the pulling speed to crystallize the molten material, and keeping the pulling speed constant after the growth is stable. After all the raw materials in the crucible are pulled out, the temperature is reduced for 12 hours, after the temperature is reduced to room temperature, the crystal growth is finished, if the temperature reduction time is short, the crystal is cracked, and the quality is poor. Compared with the existing single crystal material, the crystal generated by the method has a luminous half-height-width ratio value of the tested rare earth ions which is wider than that of the single crystal material, and can be used for tunable laser output.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (8)

1. A Czochralski method for growing rare earth ion doped silicate eutectic material is characterized in that: the chemical formula of the eutectic material is Re4xBi4(1-x)Si3O12/Bi12SiO20Wherein, the rare earth ion Re is any one of Nd, Yb, Tm, Ho, Er, Pr, Dy and Sm, and the value range of x is 0.003-0.05.
2. The eutectic material of claim 1, wherein: the raw material is Bi with the purity of 5N2O3、SiO2And Re2O3In which Bi2O3And SiO2The mass fraction ratio of (1): 3.
3. the eutectic material of claim 2, wherein: when the rare earth ion Re in the raw material is Nd, the molar ratio of Nd to Bi ions is as follows: nd: 0.003-0.1 of Bi: 1; when the rare earth ion Re is Yb, the molar ratio of Yb to Bi ions is Yb: 0.5-1 of Bi: 1; when the rare earth ion Re is Tm, the molar ratio Tm of Tm to Bi ions is as follows: and Bi is 0.02:0.98 of; when the rare earth ion Re is Ho, the molar ratio Ho of Ho to Bi ions: 0.003-0.005% of Bi: 0.995-0.997; when the rare earth ion Re is Er, the molar ratio of Er to Bi ions is Er: 0.03-0.07% of Bi: 0.97-0.93; when the rare earth ion Re is Pr, the molar ratio Pr of Pr to Bi ions is as follows: bi is 0.003-0.006: 0.994-0.997; when the rare earth ion Re is Dy, the molar ratio of Dy to Bi ions is 0.02-0.04: 0.96-0.98; when the rare earth ion Re is Sm, the molar ratio of Sm to Bi ions is Sm: 0.03-0.05% of Bi: 0.95-0.97.
4. A preparation method of a Czochralski method for growing a rare earth ion doped silicate eutectic material is characterized by comprising the following steps: the eutectic material is the eutectic material as claimed in any one of claims 1 to 3, and the specific steps are as follows:
s01, weighing the powder raw materials;
according to the mole percentage of 1: 3 weighing Bi with the purity of 5N2O3、SiO2The powder is doped with a certain amount of rare earth oxide, wherein the molar ratio of rare earth ions Re to Bi ions in the rare earth oxide is Re: and Bi is X: 1-X, wherein the value of X is 0.003-0.05, weighing, the raw material is 200-350g, and putting the raw material into an agate mortar for fully grinding to uniformly mix the raw material;
s02, pressing the blank and sintering at high temperature
Pressing the ground raw material S01 by adopting a hydraulic press, pressing the raw material into a block blank, and sintering at 480-650 ℃ for 8-17h for forming to obtain a polycrystalline raw material;
s03, charging
Placing the seed crystal, the crucible center and the coil center on the same vertical line, then placing the seed crystal, the crucible center and the coil center into a pulling furnace for growth, starting a mechanical pump for vacuum pumping, filling inert gas as protective atmosphere, and completing furnace charging;
s04, growing
Heating up, heating up within 1.5-2.8h and keeping constant temperature to ensure that the raw materials in the crucible are completely melted, wherein the growth process comprises seeding, shouldering and diameter equalization, slowly cooling to room temperature after the growth is finished, and taking out the crystal.
5. The method of claim 4, wherein: in the step S01, the grinding time of the powder raw material is 40-60 min.
6. The method of claim 4, wherein: in the step S02, the pressing pressure of the hydraulic press is 15-35MPa, and the pressing time is 5-10 min.
7. The method of claim 4, wherein: and after the growth in the step S04 is finished, the cooling time is 10-15h, so that the crystal cracking caused by the excessively high cooling rate is prevented.
8. The method of claim 4, wherein: in step S01, the rare earth ion Re in the raw material is any one of Nd, Yb, Tm, Ho, Er, Pr, Dy, and Sm, and when the rare earth ion Re is any one of the above, the molar ratio of the rare earth ion Re to the Bi ion is: nd, Bi is 0.003-0.1: 1; 0.5-1:1 of Yb and Bi; tm is 0.02: 0.98; and Ho, Bi is 0.003-0.005: 0.995-0.997; er, Bi is 0.03-0.07: 0.97-0.93; bi is 0.003-0.006: 0.994-0.997; bi is 0.02-0.04: 0.96-0.98; 0.03-0.05% of Sm and Bi: 0.95-0.97.
CN202011147283.4A 2020-10-23 2020-10-23 Czochralski method for growing rare earth ion doped silicate eutectic material and preparation method thereof Pending CN112359419A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011147283.4A CN112359419A (en) 2020-10-23 2020-10-23 Czochralski method for growing rare earth ion doped silicate eutectic material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011147283.4A CN112359419A (en) 2020-10-23 2020-10-23 Czochralski method for growing rare earth ion doped silicate eutectic material and preparation method thereof

Publications (1)

Publication Number Publication Date
CN112359419A true CN112359419A (en) 2021-02-12

Family

ID=74511916

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011147283.4A Pending CN112359419A (en) 2020-10-23 2020-10-23 Czochralski method for growing rare earth ion doped silicate eutectic material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112359419A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070108425A1 (en) * 2002-10-01 2007-05-17 The Regents Of The University Of California Nonlinear optical crystal optimized for Ytterbium laser host wavelengths
US20120199791A1 (en) * 2009-10-12 2012-08-09 Mingjie Zhou Bismuth ion sensitized rare earth germanate luminescence materials and preparation methods thereof
CN110331444A (en) * 2019-07-09 2019-10-15 同济大学 A kind of rare earth ion doped silicate eutectic material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070108425A1 (en) * 2002-10-01 2007-05-17 The Regents Of The University Of California Nonlinear optical crystal optimized for Ytterbium laser host wavelengths
US20120199791A1 (en) * 2009-10-12 2012-08-09 Mingjie Zhou Bismuth ion sensitized rare earth germanate luminescence materials and preparation methods thereof
CN110331444A (en) * 2019-07-09 2019-10-15 同济大学 A kind of rare earth ion doped silicate eutectic material and preparation method thereof

Similar Documents

Publication Publication Date Title
CN110331444B (en) Rare earth ion doped silicate eutectic material and preparation method thereof
CN110331443B (en) Rare earth ion doped germanate eutectic material and preparation method thereof
WO2021004078A1 (en) Praseodymium-doped gadolinium scandate visible waveband laser crystal and preparation method therefor
CN105198224B (en) YAG microcrystalline glass and preparation method and application thereof
CN103059860B (en) Manganese-doped yttrium aluminium garnet monocrystal material and application for same
CN109592907B (en) Boron bismuthate glass-based Ce: YAG glass ceramic for white light LED and preparation method thereof
CN107841789A (en) Yttrium aluminate visible waveband laser crystal that a kind of dysprosium terbium is co-doped with and preparation method thereof
Qiao Luminescence, energy transfer and tunable white emitting of borosilicate glass doubly doped with Tb/Sm or triply doped with Ce/Tb/Sm for white LEDs
CN110607557A (en) Spectrum-doped lead fluoride visible-band laser crystal and preparation method thereof
CN112359419A (en) Czochralski method for growing rare earth ion doped silicate eutectic material and preparation method thereof
CN100547125C (en) Y and Zn double-doped lead tungstate crystal and preparation method thereof
CN102060442A (en) Preparation method of fluorescent microcrystalline glass for white light-emitting diode (LED)
WO2022052076A1 (en) Silicate eutectic material doped with rare earth ion prepared by means of pulling process and preparation method therefor
CN104059640A (en) Preparation methods of borate fluorescent powder matrix and fluorescent powder
CN105369352A (en) Carbon-copper double-doped sapphire crystal and preparing method thereof
WO2022052078A1 (en) Rare earth ion-doped germanate eutectic material and preparation method therefor
CN106835280B (en) A kind of rare earth ion Ln3+Doping gadolinium aluminate strontium laser crystal
CN111575793A (en) Yb-doped gadolinium lanthanum silicate femtosecond laser crystal with ultra-wide emission spectral bandwidth
CN101328614A (en) Yb and Er double doping plumbous tungstate crystal conversion material and preparation thereof
CN100497759C (en) Yb and Zn double-doped lead tungstate crystal and its preparation method
JPH085753B2 (en) Terbium aluminate and its manufacturing method
CN113502530B (en) Yb, pr co-doped lead fluoride blue, green and near infrared laser crystal and preparation method and application thereof
CN110284192A (en) Infrared band laser crystal and preparation method thereof in 3 μm of er-doped scandium acid gadolinium a kind of
CN112952544B (en) Dysprosium terbium aluminum tri-doped yellow laser crystal and preparation method and application thereof
CN112251811A (en) Rare earth ion doped germanate eutectic material and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20210212