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(12) Patent Application Publication (10) Pub. No.: US 2003/0003300 A1 Korgel Et Al

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(12) Patent Application Publication (10) Pub. No.: US 2003/0003300 A1 Korgel Et Al US 20030003300A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2003/0003300 A1 KOrgel et al. (43) Pub. Date: Jan. 2, 2003 (54) LIGHT-EMITTING NANOPARTICLES AND Publication Classification METHOD OF MAKING SAME (51) Int. Cl." ............................ B32B 1700; CO9K11/00; (76) Inventors: Brian A. Korgel, Round Rock, TX HO5B 33/14 (US); Keith P. Johnston, Austin, TX (52) U.S. Cl. ......................... 428/402; 428/403; 428/690; (US) 428/917; 427/215; 313/503; 257/88 Correspondence Address: ERC B. MEYERTONS (57) ABSTRACT CONLEY, ROSE & TAYON, PC. P.O. BOX 398 AUSTIN, TX 78767-0398 (US) A method for the production of a robust, chemically stable, crystalline, passivated nanoparticle and composition con (21) Appl. No.: 10/109,578 taining the same, that emit light with high efficiencies and size-tunable and excitation energy tunable color. The meth (22) Filed: Mar. 28, 2002 ods include the thermal degradation of a precursor molecule Related U.S. Application Data in the presence of a capping agent at high temperature and elevated pressure. A particular composition prepared by the (60) Provisional application No. 60/302,594, filed on Jul. methods is a passivated Silicon nanoparticle composition 2, 2001. displaying discrete optical transitions. Patent Application Publication Jan. 2, 2003 Sheet 1 of 31 US 2003/0003300 A1 3:^*sassisssss sessia's S&* a Y f Patent Application Publication Jan. 2, 2003 Sheet 2 of 31 US 2003/0003300 A1 Fig. 2 Patent Application Publication Jan. 2, 2003 Sheet 3 of 31 US 2003/0003300 A1 S a. i.e. i.e. Fig. 4 Patent Application Publication Jan. 2, 2003 Sheet 6 of 31 US 2003/0003300 A1 62 Patent Application Publication Jan. 2, 2003 Sheet 7 of 31 US 2003/0003300 A1 * \/f) 68 N- 74 Fig. 8 72 76 Patent Application Publication Jan. 2, 2003 Sheet 8 of 31 US 2003/0003300 A1 8 3 S. Patent Application Publication Jan. 2, 2003 Sheet 10 of 31 US 2003/0003300 A1 1OO 94 1 OO Fig.11 Patent Application Publication Jan. 2, 2003 Sheet 11 of 31 US 2003/0003300 A1 4 O ": s : Energy (keV) Fig. 12 Patent Application Publication Jan. 2, 2003 Sheet 12 of 31 US 2003/0003300 A1 an au as 95 100 105 1. Binding Energy (ew 282 egg as 28s 28s 228s Binding Energy (eV) Fig. 13 Patent Application Publication Jan. 2, 2003 Sheet 13 of 31 US 2003/0003300 A1 is is . Wavenumber (cm) Fig. 14 Patent Application Publication Jan. 2, 2003 Sheet 14 of 31 US 2003/0003300 A1 y A 15 A diameter - 'f-23% f v=50 pS As 2540 A diameter (A, V 3OO 400 500 600 700 800 Wavelength (nm) Fig. 15 Patent Application Publication Jan. 2, 2003 Sheet 15 of 31 US 2003/0003300 A1 25C 300 350 400 450 500 550 600 Wavelength (rim) Fig. 16 Patent Application Publication Jan. 2, 2003 Sheet 16 of 31 US 2003/0003300 A1 O 10 1.0 2.0 3.0 4.0 5.0 Energy (eV) Fig. 17 Patent Application Publication Jan. 2, 2003 Sheet 17 of 31 US 2003/0003300 A1 g Patent Application Publication Jan. 2, 2003 Sheet 18 of 31 US 2003/0003300 A1 E. r . O) age r .9) L s r Patent Application Publication Jan. 2, 2003 Sheet 19 of 31 US 2003/0003300 A1 OZ(61-) issues Patent Application Publication Jan. 2, 2003 Sheet 20 of 31 US 2003/0003300 A1 (S)0 W s Sp cN Cd S S. er C O N O O N O O CO O O CO O D O Og O OC CC. N. CN C. r O O O O O SU 9 Up 0Ze WJON Patent Application Publication Jan. 2, 2003 Sheet 21 of 31 US 2003/0003300 A1 is is Binding Energy (eV) Fig. 22 Patent Application Publication Jan. 2, 2003 Sheet 22 of 31 US 2003/0003300 A1 Wavelength (nm) O) 500 400 3.0 - 230 is sists Energy (eV) Fig. 23 Patent Application Publication 3DO 400 500 600 700 Wavelength (nm) Patent Application Publication Jan. 2, 2003 Sheet 24 of 31 US 2003/0003300 A1 . t(s). Patent Application Publication Jan. 2, 2003 Sheet 25 of 31 US 2003/0003300 A1 12x10 A. O Three Exponential Fit 8 avg F 3.1 ns y 8 Fig. 27 3 4 C 2 O O 5 O 5 Time {ns) 1000 e b 800ss 2 . sissists 600 sa s Fig. 28 2400 E 20 50 - - Shift from 5 Og O C 0.8 e D.8 3. gs s 0.4 Fig. 29 O2 S. S5 60 S5 f 75 Wavelength (nir) Patent Application Publication Jan. 2, 2003 Sheet 26 of 31 US 2003/0003300 A1 Emission t A1 2 A2 t3 A3 Wavelength (ns) (%) (ns) (%) (ns) (%) (nm) 520 0.27 31 2.2 46 5.7 23 560 0.33 29 2.3 46 6.0 25 600 O.37 27 2.3 47 6.2 26 640 O.39 28 2.3 47 6.4 25 68O 0.42 30 2.2 46 6.3 24 Fig. 30 Patent Application Publication Jan. 2, 2003 Sheet 27 of 31 US 2003/0003300 A1 Power supply Spectrometer CCD canara Photomultiplier Fig. 31 Patent Application Publication Jan. 2, 2003 Sheet 28 of 31 US 2003/0003300 A1 {{{ }} Fig. 32 Patent Application Publication Jan. 2, 2003 Sheet 29 of 31 US 2003/0003300 A1 O. 2 (). ËE?vs.ÄgQÊ) Fig. 33 Patent Application Publication Jan. 2, 2003 Sheet 30 of 31 US 2003/0003300 A1 Y. * 2O 40 SC O Wavelength (nm) Fig. 34 Patent Application Publication Jan. 2, 2003 Sheet 31 of 31 US 2003/0003300 A1 igS 3. ÁSueuild AEISud US 2003/0003300 A1 Jan. 2, 2003 LIGHT-EMITTING NANOPARTICLES AND electronic transitions in the absorbance and photolumines METHOD OF MAKING SAME cence excitation (PLE) spectra. 0009. The wet chemical techniques used to synthesize PRIORITY CLAIM Group II-VI and III-V semiconductors have not been readily 0001. This application claims priority to Provisional applied to Group IV materials, largely due to the high Patent Application No. 60/302,594 entitled “Light-Emitting temperatures required to degrade the necessary precursors. Nanocrystals' filed on Jul. 2, 2001. Typically the temperature required to degrade the necessary Group IV precursors exceeds the boiling points of typical STATEMENT REGARDING FEDERALLY Solvents. Furthermore, the Strong covalent bonding of Si SPONSORED RESEARCH requires temperatures higher than the Group II-VI materials to achieve highly crystalline cores. Moderate progreSS has 0002 The United States Government has rights in this been made with alternative solution-phase reduction of Si invention pursuant to National Science Foundation Contract Salts and aerosol methods. These methods, however, have No. 26-1122-2OXX. produced nanocrystals with extremely broad size distribu tions. AeroSol methods have required a thick oxide coating BACKGROUND OF THE INVENTION to stabilize their structure, which has been shown recently to Significantly affect the photoluminescence (PL) energies of 0003) 1. Field of the Invention porous Si. 0004. The present invention relates to the field of nano technology. In particular, to compositions and methods of SUMMARY OF THE INVENTION making Group IV metal nanoparticles and their applications. 0010. In an embodiment Group IV metals form nanoc 0005 2. Description of the Relevant Art rystalline or amorphous particles by the thermal degradation 0006 The term “nanoparticle' generally refers to par of a precursor molecule in the presence of molecules that ticles that have an average diameter between about 1 nm to bind to the particle Surface, referred to as a capping agent at 100 nm. Nanoparticles have an intermediate size between high temperature and elevated pressure. In certain embodi individual atoms and macroscopic bulk Solids. Nanopar ments, the reaction may run under an inert atmosphere. In ticles typically have a size on the order of the Bohr exciton certain embodiments the reaction may be run at ambient radius, or the de Broglie wavelength, of the material, which preSSures. The particles may be robust, chemically stable, allows individual nanoparticles to trap individual or discrete crystalline, or amorphous and organic-monolayer passi numbers of charge carriers, either electrons or holes, or Vated, or chemically coated by a mixture of organic mol excitons, within the particle. The Spatial confinement of ecules. In one embodiment, the particles emit light in the electrons (or holes) by nanoparticles is believed to alter the ultraViolet wavelengths. In another embodiment, the par physical, optical, electronic, catalytic, optoelectronic and ticles emit light in the visible wavelengths. In other emo magnetic properties of the material. The alteration of the bodiments, the particles emit light in the near-infrared and physical properties of a nanoparticle due to confinement of the infrared wavelengths. The particles may emit light with electrons is generally referred to as quantum confinement high efficiencies. Color of the light emitted by the particles effects. may be size-tunable and excitation energy tunable. The light emission may be tuned by particle size, with Smaller par 0007 Nanoparticles may exhibit a number of unique ticles emitting higher energy than larger particles. The electronic, magnetic, catalytic, physical, optoelectronic and Surface chemistry may also be modified to tune the optical optical properties due to quantum confinement effects. For properties of the particles. In one embodiment, the Surfaces example, many nanoparticles exhibit photoluminescence may be well-passivated for light emission at higher energies effects that are Significantly greater than the photolumines than particles with Surfaces that are not well-passivated. The cence effects of macroscopic molecules having the same average diameter of the particles may be between 1 and 10 composition.
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