Nanocrystal doped matrixes

Abstract

The present invention provides matrixes doped with semiconductor nanocrystals. In certain embodiments, the semiconductor nanocrystals have a size and composition such that they absorb or emit light at particular wavelengths. The nanocrystals can comprise ligands that allow for mixing with various matrix materials, including polymers, such that a minimal portion of light is scattered by the matrixes. The matrixes of the present invention can also be utilized in refractive index matching applications. In other embodiments, semiconductor nanocrystals are embedded within matrixes to form a nanocrystal density gradient, thereby creating an effective refractive index gradient. The matrixes of the present invention can also be used as filters and antireflective coatings on optical devices and as down-converting layers. The present invention also provides processes for producing matrixes comprising semiconductor nanocrystals.

Description

CROSS REFERENCE TO RELATED APPLICATIONS

[0001] The present application is a continuation of U.S. patent application Ser. No. 11 / 034,216, filed Jan. 13, 2005, which claims the benefit of the filing dates of U.S. Provisional Patent Application No. 60 / 536,962, filed Jan. 15, 2004, and U.S. Provisional Patent Application No. 60 / 635,784, filed Dec. 15, 2004, the disclosures of which applications are incorporated by reference herein in their entireties.BACKGROUND OF THE INVENTION

[0002] 1. Field of the Invention

[0003] The present invention relates to nanocomposite matrixes, including polymeric layers comprising nanocrystals, and processes for preparing nanocrystal doped matrixes.

[0004] 2. Background Art

[0005] High performance down-converting phosphor technologies will play a prominent role in the next generation of visible light emission, including high efficiency solid-state white lighting (SSWL). In addition, such technologies are also applicable to near infrared (NIR) and infrared (...

Examples

example 1

Core / shell Nanocrystal Synthesis

[0154] Suitable nanocrystal synthesis procedures include fabricating nanocrystal samples with specific spectral characteristics matched to those prescribed by the theoretical models of the present invention. This can include fabricating nanocrystals with tunable sizes and size distributions (e.g., sizes ranging from 1-20 nm in diameter producing emission peak wavelengths tunable between 460 and 640 nm with FWHM tunable from about 15 to about 100 nm). This in turn is used to synthesize nanocrystal mixtures identified by simulations that have the optimal emission characteristics. The simulation and core / shell nanocrystal procedure is typically performed in an iterative process.

[0155] Type I core-shell nanocrystals of CdSe / ZnS (core / shell) can be synthesized by a two step process using a solution phase method, first with the fabrication of the core material followed by growth of the shell.

Core Synthesis

[0156] Stock solutions are prepared of Se powd...

example 2

ZnS Nanocrystal Synthesis

[0161] In the order listed, add the following to a 50 mL 3-neck round bottom flask:

[0162] 1. Zn(acetate)2: 76.5 mg Lot#12727BC

[0163] 2. Stearic Acid: 484 mg Lot#06615MA

[0164] 3. Tri-n-octylphosphine oxide (TOPO): 4.07 g Lot#21604LA

[0165] In a glove box prepare the following:

[0166] 3.9 g of distilled tri-n-octylphosphine (TOP) (#35-111) in 5 mL syringe;

[0167] 116.4 mg of stock solution 02-190 (bis(trimethylsilyl)sulfide (TMS2S):TOP) in 1 mL syringe; and

[0168] One 40 mL septa cap vial with 5.0 mL of MeOH

[0169] Place reactor under vacuum

[0170] Heat to 120° C.

[0171] Once at 120° C., allow to sit for 20 minutes

[0172] Place reactor under argon

[0173] Slowly inject TOP from 5 mL syringe

[0174] Change set point temperature to 250° C.

[0175] Once at 250° C., immediately inject the stock solution 02-190 (bis(trimethylsilyl)sulfide (TMS2S):TOP) from 1 mL syringe

[0176] Grow with temperature at 250° C. for 2 minutes

[0177] Remove the heating mantle and allo...

example 3

Carboxylic Acid-Silicone Ligand Synthesis

[0182] General Methods

[0183] All manipulations were carried out with strict exclusion of air and moisture by using Schlenk technique under an atmosphere of dry nitrogen, unless otherwise stated. THF, toluene, chloroform-d1 and toluene-d8 were dried over activated 4 A Molecular Sieves and de-gassed by three freeze-pump-thaw cycles. 4-pentenoic acid and 1,1,1,3,5,5,5-heptamethyltrisiloxane were purchased from Aldrich (St. Louis, Mo.), distilled and stored in a storage flask using Schlenk technique before use. Heptamethyl cyclotetrasiloxane and 1,1,1,3,3,5,5-heptamethyl trisiloxane were purchased from Gelest (Morrisville, Pa.), distilled and stored in a storage flask using Schlenk technique before use. Karstedt's catalyst or platinum divinyl tetramethyl disiloxane complex, 2.1 to 2.4% in xylenes, was purchased from Gelest, stored in the glove box and used without further purification. All products were stored in the glove box. NMR chemical sh...

CROSS REFERENCE TO RELATED APPLICATIONS

[0001] The present application is a continuation of U.S. patent application Ser. No. 11 / 034,216, filed Jan. 13, 2005, which claims the benefit of the filing dates of U.S. Provisional Patent Application No. 60 / 536,962, filed Jan. 15, 2004, and U.S. Provisional Patent Application No. 60 / 635,784, filed Dec. 15, 2004, the disclosures of which applications are incorporated by reference herein in their entireties.BACKGROUND OF THE INVENTION

[0002] 1. Field of the Invention

[0003] The present invention relates to nanocomposite matrixes, including polymeric layers comprising nanocrystals, and processes for preparing nanocrystal doped matrixes.

[0004] 2. Background Art

[0005] High performance down-converting phosphor technologies will play a prominent role in the next generation of visible light emission, including high efficiency solid-state white lighting (SSWL). In addition, such technologies are also applicable to near infrared (NIR) and infrared (...

Examples

example 1

Core / shell Nanocrystal Synthesis

[0154] Suitable nanocrystal synthesis procedures include fabricating nanocrystal samples with specific spectral characteristics matched to those prescribed by the theoretical models of the present invention. This can include fabricating nanocrystals with tunable sizes and size distributions (e.g., sizes ranging from 1-20 nm in diameter producing emission peak wavelengths tunable between 460 and 640 nm with FWHM tunable from about 15 to about 100 nm). This in turn is used to synthesize nanocrystal mixtures identified by simulations that have the optimal emission characteristics. The simulation and core / shell nanocrystal procedure is typically performed in an iterative process.

[0155] Type I core-shell nanocrystals of CdSe / ZnS (core / shell) can be synthesized by a two step process using a solution phase method, first with the fabrication of the core material followed by growth of the shell.

Core Synthesis

[0156] Stock solutions are prepared of Se powd...

example 2

ZnS Nanocrystal Synthesis

[0161] In the order listed, add the following to a 50 mL 3-neck round bottom flask:

[0162] 1. Zn(acetate)2: 76.5 mg Lot#12727BC

[0163] 2. Stearic Acid: 484 mg Lot#06615MA

[0164] 3. Tri-n-octylphosphine oxide (TOPO): 4.07 g Lot#21604LA

[0165] In a glove box prepare the following:

[0166] 3.9 g of distilled tri-n-octylphosphine (TOP) (#35-111) in 5 mL syringe;

[0167] 116.4 mg of stock solution 02-190 (bis(trimethylsilyl)sulfide (TMS2S):TOP) in 1 mL syringe; and

[0168] One 40 mL septa cap vial with 5.0 mL of MeOH

[0169] Place reactor under vacuum

[0170] Heat to 120° C.

[0171] Once at 120° C., allow to sit for 20 minutes

[0172] Place reactor under argon

[0173] Slowly inject TOP from 5 mL syringe

[0174] Change set point temperature to 250° C.

[0175] Once at 250° C., immediately inject the stock solution 02-190 (bis(trimethylsilyl)sulfide (TMS2S):TOP) from 1 mL syringe

[0176] Grow with temperature at 250° C. for 2 minutes

[0177] Remove the heating mantle and allo...

example 3

Carboxylic Acid-Silicone Ligand Synthesis

[0182] General Methods

[0183] All manipulations were carried out with strict exclusion of air and moisture by using Schlenk technique under an atmosphere of dry nitrogen, unless otherwise stated. THF, toluene, chloroform-d1 and toluene-d8 were dried over activated 4 A Molecular Sieves and de-gassed by three freeze-pump-thaw cycles. 4-pentenoic acid and 1,1,1,3,5,5,5-heptamethyltrisiloxane were purchased from Aldrich (St. Louis, Mo.), distilled and stored in a storage flask using Schlenk technique before use. Heptamethyl cyclotetrasiloxane and 1,1,1,3,3,5,5-heptamethyl trisiloxane were purchased from Gelest (Morrisville, Pa.), distilled and stored in a storage flask using Schlenk technique before use. Karstedt's catalyst or platinum divinyl tetramethyl disiloxane complex, 2.1 to 2.4% in xylenes, was purchased from Gelest, stored in the glove box and used without further purification. All products were stored in the glove box. NMR chemical sh...

Images