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Synthesis of multinary chalcogenide nanoparticles comprising cu, zn, sn, s, and se

A nanoparticle and particle technology, applied in the field of multi-component chalcogenide CZTSSe nanoparticles4, can solve the problems of slow progress of solar cells

Inactive Publication Date: 2012-05-16
PURDUE RES FOUND INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are problems with these deposition methods for high-throughput manufacturing, such as Cu(In,Ga)Se-based 2 The slow progress in the mass production of solar cells is evidenced by

Method used

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  • Synthesis of multinary chalcogenide nanoparticles comprising cu, zn, sn, s, and se
  • Synthesis of multinary chalcogenide nanoparticles comprising cu, zn, sn, s, and se
  • Synthesis of multinary chalcogenide nanoparticles comprising cu, zn, sn, s, and se

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Experimental program
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Effect test

Embodiment 1-C

[0091] The synthesis of embodiment 1-CZTS nanoparticles

[0092] In the synthesis of exemplary CZTS nanoparticles, copper(II) acetylacetonate (1.5mmol; 99.99%, Aldrich), zinc acetylacetonate (0.75mmol, 99.995%, Aldrich), and bis(acetylacetonate) A mixture of tin(IV) bromide (0.75 mmol; 98%, Aldrich) and 10 ml oleylamine (technical grade, Aldrich) was added to a 100 ml three-necked flask connected to Schreck technology. The mixture was heated to about 130 °C under vacuum, degassed for 30 min, and sparged with Ar several times. After raising the temperature to 200°C-245°C, 3ml of a 1M sulfur solution (in oleylamine) was injected through the third neck. After injection, the reaction was allowed to mix for 30 minutes to completion. The heating mantle was then removed and the mixture was cooled to about 80°C. The resulting nanocrystals were collected by centrifugation in a 3:1 mixture of isopropanol and toluene. The precipitate was then redispersed in about 40 ml of toluene to ...

Embodiment 2

[0095] Example 2 - Synthesis of Cu-deficient, Zn-enriched CZTS nanoparticles

[0096] By varying the relative amounts of metal precursors used in the synthesis, the ratio of Cu:Zn:Sn in the CZTS nanoparticles can be varied. In one embodiment, copper(II) acetylacetonate (0.75 mmol; 99.99%, Aldrich), zinc acetylacetonate (0.75 mmol; 99.995%, Aldrich), and bis(acetylacetonate)tin dibromide 10 ml of oleylamine (technical grade, Aldrich) of the mixture of (IV) (0.5 mmol; 98%, Aldrich) was added to a 100 ml three-neck flask connected to Schleck technology. The mixture was heated to about 130 °C under vacuum, degassed for 30 min, and sparged with Ar several times. After raising the temperature to about 235°C, 2 ml of a 1M sulfur solution (in oleylamine) was injected through the third neck. After injection, the reaction was allowed to mix for 30 minutes to completion. The heating mantle was then removed and the mixture was cooled to about 80°C. The resulting nanocrystals were coll...

Embodiment 3

[0097] Example 3 - Synthesis of CZTS nanoparticles using non-coordinating solvents

[0098] By using the required amount of coordinating ligands (such as amines, carboxylic acids, ethers, phosphines, phosphonic acids, and thiols), the synthesis of CZTS nanoparticles can use non-coordinating solvents (such as and alkenes). For example, a non-coordinating solvent such as octadecene can be used with oleic acid as a coordinating ligand.

[0099] More specifically, 10 ml of octadecene (technical grade, Aldrich) was mixed with 1.58 ml of oleic acid (technical grade, Aldrich) to form a solution of reconstituted solvent, to which copper (II) acetylacetonate (1 mmol; 99.99%, Aldrich), zinc acetylacetonate (0.5 mmol; 99.995%, Aldrich), and bis(acetylacetonate)tin(IV) dibromide (0.5 mmol; 98%, Aldrich). The resulting precursor solution was added to a 100 ml three-necked flask connected to Schleck technology. The reaction product was heated to about 130°C under vacuum, degassed for 30 ...

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Abstract

Nanoparticle compositions and methods for synthesizing multinary chalcogenide CZTSSe nanoparticles containing Cu, Zn, and Sn in combination with S, Se or both are described. The nanoparticles may be incorporated into one or more ink solutions alone or in combination with other chalcogenide-based particles to make thin films useful for photovoltaic applications, including thin films from multilayer particle films having a composition profile. The composition and stoichiometry of the thin films may be further modified by subjecting the particle films to gas or liquid phase chalcogen exchange reactions.

Description

[0001] related application [0002] This application claims priority under 35 U.S.C. §119(e) to U.S. Provisional Patent Application No. 61 / 181,160, filed May 26, 2009, which is incorporated herein by reference in its entirety. technical field [0003] The present invention relates to multi-component chalcogenide CZTSSe nanoparticles containing Cu, Zn, Sn, S and Se (i.e. Cu 2 ZnSn(S y , Se 1-y ) 4 , wherein 0≤y≤1) compositions, and their synthesis and use methods. Nanoparticles can be used to make thin films useful in optoelectronic applications. Background technique [0004] Among the various semiconducting nanomaterials studied for optoelectronic applications, one of the more promising candidates for low-cost solar cells is chalcopyrite nanocrystals I-III-VI 2 family, especially Cu(In,Ga)Se 2 (3, 5, 6). Based on Cu(In,Ga)Se 2 The photon-to-electron conversion efficiency of thin-film solar cells is as high as 19.9% ​​(13). However, due to supply constraints and incr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B82B3/00H01L31/042
CPCH01L21/02601H01L31/0322C23C18/127H01L21/02568H01L31/0324H01L21/02628Y02E10/50Y02E10/541H01L21/0256H01L21/02614H01B1/10C01B19/002
Inventor R.阿格拉瓦尔H.W.希尔豪斯郭起洁
Owner PURDUE RES FOUND INC
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