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  • The Effect of Annealing Conditions and Concentration on 5 D 3 7 F J Emission in Terbium-doped Sol-gel Glasses * Colleen Gillespie and Dan Boye, Davidson
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The Effect of Annealing Conditions and Concentration on 5 D 3 7 F J Emission in Terbium-doped Sol-gel Glasses * Colleen Gillespie and Dan Boye, Davidson College, Davidson, NC Ann Silversmith, Hamilton College, Clinton, NY Abstract Sol-gel glasses have optical properties similar to those of traditional melt glasses, but are appealing because they can hold a higher concentration of dopants due to their lower processing temperatures. In silicate sol-gel doped with trivalent terbium, the intensity of fluorescence from the 5 D 3 level to the 7 F J (J = 0…6) ground state manifold levels is highly dependent on both terbium concentration and annealing conditions. 5 D 3 emission is observed in glasses annealed at 750C and increases in intensity with increasing annealing time and with higher annealing temperature. The relative intensity of emission from the 5 D 3 state decreases with increasing Tb 3+ concentration. A cross-relaxation process involving two nearby Tb 3+ ions depopulates the 5 D 3 level and causes this concentration quenching. •Project supported by a grant from the NSF-NRI program 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 Energy (1000cm - 1 ) 7 F 6 5 4 3 7 F 0 1 2 5 D 4 5 D 3 414n m 436n m 460n m 490nm 545nm 590nm 620nm 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 Energy (1000cm - 1 ) 7 F 6 5 4 3 7 F 0 1 2 5 D 4 5 D 3 Conclusions Terbium Energy Levels Results: Annealing Conditions Theory: Concentration Dependence Results: Concentration Dependence Dissolve 11.8 mg of terbium nitrate (Tb(NO 3 ) 3 *5H 2 O) and 20.3 mg of aluminum nitrate (Al(NO 3 ) 3 *9H 2 O) in 7.8 mL deionized water. Add 20 μL concentrated nitric acid and 4.00 mL TMOS (tetramethylorthosilicate, 99%) to solution and stir for 10 minutes Put sol into 4 tightly capped polystyrene disposable test tubes Gel at room temperature for 72 hours Ramp at 5ºC/hr to 60ºC, then sit for 48 hours Ramp at 5ºC/hr to 90ºC, then sit for 48 hours Ramp at 2ºC/hr to 110ºC, then sit for 48 hours Let cool to room temperature This is a partial energy level diagram of trivalent terbium, with labeled transitions corresponding to observed fluorescence lines. The samples were excited with 240 nm excitation light. The 5 D 4 7 F 5 transition dominates the emission spectrum and produces a green color. A cross-relaxation process involving two Tb 3+ ions depopulates the 5 D 3 level and reduces 5 D 3 emission intensity. At higher terbium concentrations, the terbium atoms are closer together, so there is stronger cross-relaxation. Therefore, we predict that as terbium concentration increases, the intensity of the 5 D 3 peak will decrease. After the sample is taken out of the oven, it begins to reabsorb hydroxyl groups, and the 5 D 3 peak begins to shrink. Here is a close up of the 5 D 3 peaks at three consecutive times. This decay is enhanced by increasing the hydroxyl concentration by putting the sample in water for a few minutes. • We determined that heating the samples to 900ºC with a 12 hour dwell gives optimal optical properties without damaging the sample. • We confirmed that the 5 D 3 emission intensity decreases with increasing terbium concentration • Now that we have determined the best protocol for processing these samples, we can use our knowledge to begin working with erbium-doped sol-gels. Motivation: Sol-gel glasses Sol-gel synthesis is a low temperature was to prepare optically transparent materials. Because the sol-gel is prepared at room temperature, it is easy to include metallic, organic, and inorganic additives. The optical properties of a sol-gel that has been heated to ~1000ºC are similar to those of traditional melt glasses, but since this temperature is below the melting point of the material, the sol-gels can hold more dopants than melt glasses. Sol-gels with rare earth ions as dopants are used in phosphors, solid-state lasers, and amplifiers. We can use the optical properties of these materials to characterize the interactions between the dopants and the surrounding material. Theory: Annealing conditions Hydroxyl groups are present in the sol-gel materials. They have an absorption band between 2000 and 4000 cm -1 . This allows electrons in the 5 D 3 level to relax to the 5 D 4 level by losing energy to another hydroxyl group combined with a lattice vibrational mode. This means that there is virtually no fluorescence from the 5 D 3 level. However, the number of hydroxyl grounds in the material can be significantly reduced by annealing the samples at a high temperature. Consequently, the 5 D 3 emission becomes comparable to 5 D 4 emission. When the samples are taken to 750ºC, the 5 D 3 peak becomes detectable. Taking the samples to higher temperatures and for longer dwell times at those temperatures, the intensity of the 5 D 3 peak becomes stronger. However, if the samples are annealed at too high a temperature, they can start to crystallize or crack. Therefore, we wanted to find an ideal annealing temperature and time to have a high 5 D 3 emission without any damage to the sample. I heated the sample to 800, 900, and 1000ºC for various dwell times. I then plotted the ratio of the 5 D 3 7 F 4 transition to the 5 D 4 7 F 6 transition. At higher temperatures and for higher dwell times, the ratio increases. The sample shattered after being at 1000ºC for 4 hours. Picture of Samples Which sample looks bluer? So, which sample has the lower concentration? The sample on the left has a concentration of 0.5%, and the one on the right is 0.1%. The 0.5% sample has very little emission from the 5 D 3 level (blue light) while the 0.1% sample has a substantial amount of emission from this level, and therefore looks blue-ish. 0.0E+00 1.0E+07 2.0E+07 3.0E+07 4.0E+07 5.0E+07 6.0E+07 400 420 440 460 480 500 w avelength (nm ) Fluorescence 0 m ins 13 m ins 25 m ins 3 m ins in H2O Plotting spectra of four different concentrations, it is clear that 5 D 3 emission decreases as terbium concentration increases. Exposure to Humidity Sol-gel Recipe 0 0.5 1 1.5 2 2.5 3 3.5 0 2 4 6 8 10 12 14 Dw elltim e athighesttem perature Ratio 800 900 1000 New sam ple concentration dependence -1.0E+07 4.0E+07 9.0E+07 1.4E+08 1.9E+08 2.4E+08 2.9E+08 400 450 500 550 600 650 W avelength (nm ) Fluorescence (arb.units) 0.05% 0.10% 0.20% 0.50%

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  • The Effect of Annealing Conditions and Concentration on 5D3 7FJ Emission in Terbium-doped Sol-gel Glasses *

    Colleen Gillespie and Dan Boye, Davidson College, Davidson, NCAnn Silversmith, Hamilton College, Clinton, NYAbstract

    Sol-gel glasses have optical properties similar to those of traditional melt glasses, but are appealing because they can hold a higher concentration of dopants due to their lower processing temperatures. In silicate sol-gel doped with trivalent terbium, the intensity of fluorescence from the 5D3 level to the 7FJ (J = 06) ground state manifold levels is highly dependent on both terbium concentration and annealing conditions. 5D3 emission is observed in glasses annealed at 750C and increases in intensity with increasing annealing time and with higher annealing temperature. The relative intensity of emission from the 5D3 state decreases with increasing Tb3+ concentration. A cross-relaxation process involving two nearby Tb3+ ions depopulates the 5D3 level and causes this concentration quenching.

    Project supported by a grant from the NSF-NRI programConclusionsTerbium Energy LevelsResults:Annealing Conditions Theory: Concentration DependenceResults: Concentration Dependence

    Dissolve 11.8 mg of terbium nitrate (Tb(NO3)3*5H2O) and 20.3 mg of aluminum nitrate (Al(NO3)3*9H2O) in 7.8 mL deionized water.Add 20 L concentrated nitric acid and 4.00 mL TMOS (tetramethylorthosilicate, 99%) to solution and stir for 10 minutesPut sol into 4 tightly capped polystyrene disposable test tubesGel at room temperature for 72 hoursRamp at 5C/hr to 60C, then sit for 48 hoursRamp at 5C/hr to 90C, then sit for 48 hoursRamp at 2C/hr to 110C, then sit for 48 hoursLet cool to room temperatureThis is a partial energy level diagram of trivalent terbium, with labeled transitions corresponding to observed fluorescence lines. The samples were excited with 240 nm excitation light. The 5D4 7F5 transition dominates the emission spectrum and produces a green color.A cross-relaxation process involving two Tb3+ ions depopulates the 5D3 level and reduces 5D3 emission intensity. At higher terbium concentrations, the terbium atoms are closer together, so there is stronger cross-relaxation. Therefore, we predict that as terbium concentration increases, the intensity of the 5D3 peak will decrease.After the sample is taken out of the oven, it begins to reabsorb hydroxyl groups, and the 5D3 peak begins to shrink. Here is a close up of the 5D3 peaks at three consecutive times. This decay is enhanced by increasing the hydroxyl concentration by putting the sample in water for a few minutes. We determined that heating the samples to 900C with a 12 hour dwell gives optimal optical properties without damaging the sample. We confirmed that the 5D3 emission intensity decreases with increasing terbium concentration Now that we have determined the best protocol for processing these samples, we can use our knowledge to begin working with erbium-doped sol-gels.

    Motivation: Sol-gel glasses

    Sol-gel synthesis is a low temperature was to prepare optically transparent materials. Because the sol-gel is prepared at room temperature, it is easy to include metallic, organic, and inorganic additives. The optical properties of a sol-gel that has been heated to ~1000C are similar to those of traditional melt glasses, but since this temperature is below the melting point of the material, the sol-gels can hold more dopants than melt glasses. Sol-gels with rare earth ions as dopants are used in phosphors, solid-state lasers, and amplifiers. We can use the optical properties of these materials to characterize the interactions between the dopants and the surrounding material.Theory:Annealing conditionsHydroxyl groups are present in the sol-gel materials. They have an absorption band between 2000 and 4000 cm-1. This allows electrons in the 5D3 level to relax to the 5D4 level by losing energy to another hydroxyl group combined with a lattice vibrational mode. This means that there is virtually no fluorescence from the 5D3 level. However, the number of hydroxyl grounds in the material can be significantly reduced by annealing the samples at a high temperature. Consequently, the 5D3 emission becomes comparable to 5D4 emission.

    When the samples are taken to 750C, the 5D3 peak becomes detectable. Taking the samples to higher temperatures and for longer dwell times at those temperatures, the intensity of the 5D3 peak becomes stronger. However, if the samples are annealed at too high a temperature, they can start to crystallize or crack. Therefore, we wanted to find an ideal annealing temperature and time to have a high 5D3 emission without any damage to the sample.I heated the sample to 800, 900, and 1000C for various dwell times. I then plotted the ratio of the 5D3 7F4 transition to the 5D4 7F6 transition. At higher temperatures and for higher dwell times, the ratio increases. The sample shattered after being at 1000C for 4 hours.Picture of SamplesWhich sample looks bluer? So, which sample has the lower concentration?

    The sample on the left has a concentration of 0.5%, and the one on the right is 0.1%. The 0.5% sample has very little emission from the 5D3 level (blue light) while the 0.1% sample has a substantial amount of emission from this level, and therefore looks blue-ish.Plotting spectra of four different concentrations, it is clear that 5D3 emission decreases as terbium concentration increases.Exposure to HumiditySol-gel Recipe

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The Gillespie Gazette · 2020. 12. 6. · The Gillespie Gazette The Gillespie Center, 2590 Commerce Boulevard, Mound, MN 55364 952-472-6501 e-mail: [email protected] Gillespie

ROBERT GILLESPIE

CAROLINA ANDREA ADAROS BOYE - Alianza Chilena de

Preparasi dan Karakterisasi Komposit Terbium Tetraetilena

Boye - Epistemic Meaning

Kayla Boye Performance Resume 2016d284f45nftegze.cloudfront.net/kaylaboye/Kayla_Boye_Performance_Resume_2016.pdfKayla Boye ACTRESS, DANCER, SINGER, CHOREOGRAPHER | [email protected]

Aaron Gillespie

Boye Open Intranet

linda boye

J boye | web strategy, v1.00

Social governance j boye 2014

Spectroscopic and Thermo-gravimetric Analysis of Terbium

Kayla Boye EMCd284f45nftegze.cloudfront.net/kaylaboye/Kayla_Boye... · 2017-12-12 · Kayla Boye EMC ACTRESS, DANCER, SINGER, CHOREOGRAPHER | [email protected] | 330-647-9383 Height:

A ketone functionlized luminescent terbium metal … ketone functionlized luminescent terbium metal-organic framework for sensing of small molecules Zhiyong Guo,a aXuezhi Song,b Huaping

Terbium-mediated Footprinting Probes a Catalytic Conformational

Portfolio niu boye

JAMES NII BOYE BANNERMAN.pdf

5.48 Acres Gillespie 5.48 Gillespie County, Texas Texas

REMARKABLE INFLUENCE OF TERBIUM CATIONS … INFLUENCE OF TERBIUM CATIONS ON THE MAGNETIC PROPERTIES OF COBALT FERRITE NANOPARTICLES Tahmineh Sodaee*, Ali Ghasemi**, Ebrahim Paimozd

Luminescent Terbium/Europium Chelates-Based Silica ...Luminescent Terbium/Europium Chelates-Based Silica Nanoparticles : Stability and Incorporation Efficiency measured by Radioactive

Efficient Phosphodiester Hydrolysis by Luminescent Terbium

Location of Terbium Binding Sites on Acetylcholine Receptor

Karin Boye - Kalocaína

Dizzy gillespie

Kayla Boye EMC - d284f45nftegze.cloudfront.netd284f45nftegze.cloudfront.net/kaylaboye/Kayla_Boye... · Kayla Boye EMC ACTRESS, DANCER, SINGER, CHOREOGRAPHER | [email protected]

PENINGKATAN EFISIENSI PEMISAHAN RADIOISOTOP TERBIUM …

Grow Gillespie Action Plan Gillespie,IL

Sam Gillespie

J boye boly

L1839 Gillespie

Boye Open Intranet

Luminescent Terbium Inorganic

James Gillespie

Boye Tranum

Karin Boye Sällskapet Medlemsblad 1 2016