CN101209900A - Neodymium-doped yttrium-fluoride nanocrystalline transparent glass ceramic with high stimulated emission cross section and preparation thereof - Google Patents
Neodymium-doped yttrium-fluoride nanocrystalline transparent glass ceramic with high stimulated emission cross section and preparation thereof Download PDFInfo
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- CN101209900A CN101209900A CNA2006101353909A CN200610135390A CN101209900A CN 101209900 A CN101209900 A CN 101209900A CN A2006101353909 A CNA2006101353909 A CN A2006101353909A CN 200610135390 A CN200610135390 A CN 200610135390A CN 101209900 A CN101209900 A CN 101209900A
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Abstract
The invention discloses Nd-doped yttrium fluoride nanocrystalline transparent glass ceramic with high cross sections of stimulated emission and the preparation method thereof, which relates to the field of laser material. The components of glass ceramic are (mole ratio): 44SiO2-28Al 2O3-xYF3-yLiF-zNdF3 (x=13-18, z=0.01-2.0, y= (28-x-z)). The invention is prepared by melt-spinning technique. Corresponding to the transition emission peak of <4>F3/2-< 4>IJ (J=9/2, 11/2, 13/2), the glass ceramic has obvious stark effect. The transition emission peak of <4>F3/2-< 4>I 11/2 can be up to 15.53 multiplied by 10<-20>cm<2>, which is much higher than that of the existing applied Nd-doped laser glass.
Description
Technical field
The present invention relates to the solid laser material field, especially relate to a kind of Nd-doped glass ceramic and preparation technology thereof with high stimulated emission cross section.
Background technology
Solid laser material commonly used at present generally is crystal or glass.The laser crystals spectrum property is more excellent, and shortcoming is that the preparation difficulty is big, cost is high; Compare with laser crystals, glass material prepares easily, and is with low cost, but because its spectral line broad, emission and absorption cross is little, laser starting of oscillation threshold value height, output efficiency is low generally speaking.Glass-ceramic is that glassy phase passes through partially-crystallized getting, and makes crystal particle scale below 30nm and be uniformly distributed in the glass basis by the control crystallization, can obtain transparent glass-ceramic.The transparent glass ceramics of fluoride crystalline phase is a kind of new pattern laser material in the oxide glass matrix, has great application prospect in optical communication, optical information field.Up to the present, the neodymium-doped fluoride crystalline phase glass-ceramic of having reported in the world, its
1F
3/2→
1I
11/2The stimulated emission cross section of transition is up to 6.88 * 10
-20Cm
2, corresponding material component is SiO
2-Al
2O
3-PbF
2-CdF
2-YF
3[with reference to M.Abril et al, J.Appl.Phys.95,5271 (2004)].But such material has reduced its industrial application value owing to containing deleterious plumbous fluoride and cadmium fluoride.The present invention proposes a kind of new nanocrystalline glass-ceramic and preparation technology thereof of neodymium-doped fluorinated yttrium, by adjusting material component, can make material
4F
3/2→
4I
11/2Transition has very high stimulated emission cross section, has application prospect as the solid laser material of 1.06 microns emissions.
Summary of the invention
The present invention proposes a kind of component and preparation technology thereof of neodymium-doped fluorinated yttrium nano crystal transparent glass ceramic, and purpose is to prepare Stability Analysis of Structures, solid laser material that stimulated emission cross section is high.
Transparent glass ceramics component of the present invention is (mol ratio): 44SiO
2-28Al
2O
3-xYF
3-yLiF-zNdF
3(x=13～18, z=0.01～2.0, y=(28-x-z)).
The present invention adopts and to be prepared as follows technology: with powder raw material according to certain set of dispense than grinding even being placed in the crucible, in resistance furnace, be heated to 1300-1500 ℃ after insulation 1-5 hour, then, glass melt is poured into fast in the copper mold of 300 ℃ of preheatings and is shaped; The glass that obtains is put into resistance furnace annealing to eliminate internal stress; Glass continuation after the annealing made it to take place partially-crystallized at 550-750 ℃ of heat tracing 1-10 hour, obtain blue transparent glass ceramics.
Adopt above forerunner's glass ingredient and preparation technology, successfully obtain in the oxide glass matrix, to contain the nanocrystalline glass-ceramic of equally distributed neodymium-doped yttrium oxide.On the room temperature fluorescence emission spectrum of glass-ceramic, corresponding to
4F
3/2→
1I
1Tangible Stark splitting appears in the emission peak of (J=9/2,11/2,13/2) transition, as shown in drawings.The luminescent properties of material and its component are closely related, by the adjustment component,
4F
3/2→
1I
11/2The stimulated emission cross section of transition can be up to 15.53 * 10
-20Cm
2, be much higher than neodymium-doped laser glass (its that has obtained application at present
1F
3/2→
1I
11/2The emission cross section of transition is in 2.7-4.3 * 10
20Cm
2Scope).
Simple, not high, with low cost, the heterotypic material that is easy to get of equipment requirements of glass-ceramic preparation technology of the present invention, Stability Analysis of Structures and can obtain very high stimulated emission cross section, may develop becomes a kind of 1.06 microns novel emission solid laser materials.
Description of drawings
Accompanying drawing is a glass-ceramic
4F
3/2→
4I
1The room temperature fluorescence emission spectrum of transition.
The specific examples mode
Example 1: with analytically pure SiO
2, Al
2O
3, LiF, YF
3With purity be 99.99% NdF
3Powder is pressed 2.0NdF
3: 44SiO
2: 28Al
2O
3: 10LiF: 16YF
3The accurate weighing of the proportioning of (mol ratio) is placed in the agate mortar, make its uniform mixing more than grinding half an hour, and be placed in the platinum crucible, in program control high temperature box type resistance furnace, be heated to 1400 ℃ after insulation 1.5 hours, then, glass melt is poured into fast in the copper mold of 300 ℃ of preheatings and be shaped; The glass that obtains is put into resistance furnace, 500 ℃ of annealing after 2 hours furnace cooling to eliminate internal stress; Glass after the annealing after 2 hours, is obtained transparent glass ceramics blue, that mix 2.0% neodymium ion 570 ℃ of insulations.Transmission electron microscope studies show that the YF that is of a size of 20-30nm is in a large number arranged in this glass-ceramic
3Uniform crystal particles is distributed in the oxide glass matrix.Sample measures the room temperature emission spectrum through surface finish with the FLS920 fluorescence spectrophotometer, as calculated,
4F
3/2→
4I
11/2The stimulated emission cross section of transition is 5.49 * 10
20Cm
2, luminous quantum efficiency is 67%.
Example 2: with analytically pure SiO
2, Al
2O
3, LiF, YF
3With purity be 99.99% NdF
3Powder is pressed 1.0NdF
3: 44SiO
2: 28Al
2O
3: 10LiF: 17YF
3The accurate weighing of the proportioning of (mol ratio) after the preparation and heat treatment process identical with example 1, obtains transparent glass ceramics blue, that mix 1.0% neodymium ion.Sample measures the room temperature emission spectrum through surface finish with the FLS920 fluorescence spectrophotometer, as calculated,
1F
3/2→
1I
11/2The stimulated emission cross section of transition is 7.83 * 10
-20Cm
2, luminous quantum efficiency is 78%.
Example 3: with analytically pure SiO
2, Al
2O
3, LiF, YF
3With purity be 99.99% NdF
3Powder is pressed 0.1NdF
3: 44SiO
2: 28Al
2O
3: 10LiF: 17.9YF
3The accurate weighing of the proportioning of (mol ratio) after the preparation and heat treatment process identical with example 1, obtains nattier blue, as to mix 0.1% neodymium ion transparent glass ceramics.Sample measures the room temperature emission spectrum through surface finish with the FLS920 fluorescence spectrophotometer, as calculated,
4F
3/2→
4I
11/2The stimulated emission cross section of transition reaches 15.53 * 10
-20Cm
2, luminous quantum efficiency reaches 95%.
Claims (3)
1. neodymium-doped yttrium-fluoride nanocrystalline transparent glass ceramic with high stimulated emission cross section is characterized in that: this glass-ceramic component is (mol ratio): 44SiO
2-28Al
2O
3-xYF
3-yLiF-zNdF
3, x=13～18 wherein, z=0.01～2.0, y=(28-x-z).
2. the preparation method of the neodymium-doped yttrium-fluoride nanocrystalline transparent glass ceramic with high stimulated emission cross section of a claim 1 is characterized in that: adopt the preparation of melt supercooled method.
3. preparation method as claimed in claim 2 is characterized in that: adopt SiO
2, Al
2O
3, NaF, YF
3, and NdF
3Powder is as raw material, mixes post-heating insulation 1-5 hour after 1300-1500 ℃, then, glass melt poured into fast in the copper mold of 300 ℃ of preheatings and is shaped; The glass that obtains is put into resistance furnace annealing to eliminate internal stress; Glass after the annealing continued at 550-750 ℃ of heat tracing 1-10 hour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101353909A CN101209900A (en) | 2006-12-27 | 2006-12-27 | Neodymium-doped yttrium-fluoride nanocrystalline transparent glass ceramic with high stimulated emission cross section and preparation thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101353909A CN101209900A (en) | 2006-12-27 | 2006-12-27 | Neodymium-doped yttrium-fluoride nanocrystalline transparent glass ceramic with high stimulated emission cross section and preparation thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101209900A true CN101209900A (en) | 2008-07-02 |
Family
ID=39610179
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006101353909A Pending CN101209900A (en) | 2006-12-27 | 2006-12-27 | Neodymium-doped yttrium-fluoride nanocrystalline transparent glass ceramic with high stimulated emission cross section and preparation thereof |
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|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092951A (en) * | 2009-12-11 | 2011-06-15 | 中国科学院福建物质结构研究所 | Transparent glass ceramic material for ultraviolet excited white LED and preparation technique thereof |
-
2006
- 2006-12-27 CN CNA2006101353909A patent/CN101209900A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092951A (en) * | 2009-12-11 | 2011-06-15 | 中国科学院福建物质结构研究所 | Transparent glass ceramic material for ultraviolet excited white LED and preparation technique thereof |
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Open date: 20080702 |