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Atypical kesterite compositions

A technology of kesterite and composition, which is applied in the field of preparing CZTS film, and can solve the problems of severe toxicity

Inactive Publication Date: 2013-01-30
EI DU PONT DE NEMOURS & CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, hydrazine is a highly reactive and potentially explosive solvent, which is described in the "Merck Index" as "very toxic"

Method used

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  • Atypical kesterite compositions
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  • Atypical kesterite compositions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090]

[0091]Zinc diethyldithiocarbamate (0.5919g, 1.635mmol), copper (II) dimethyldithiocarbamate (0.9930g, 3.267mmol) and di-n-butyltin sulfide (0.4506g, 1.701mmol ) into a 40 mL amber vial equipped with a stir bar. 4-tert-butylpyridine (4.4144 g) was added and the resulting mixture was stirred to homogeneity. Then 0.0520 g (1.621 mmol) of elemental sulfur was added. The reaction mixture was stirred at room temperature for ~12 hours, then at the first heating temperature of 105°C for ~40 hours. The reaction mixture was then stirred at a second heating temperature of 190°C for ~8 hours. SLG-coated substrate 1A was prepared by drop coating according to the following method: While maintaining at 105°C under agitation, a small portion of the formulation was drawn into a pipette and spread evenly on a substrate that was also heated to 105°C superior. The coatings on the SLG slides were then dried in a drying oven by increasing the hot plate temperature from 105°C to 170°...

Embodiment 2

[0095]

[0096] In a dry box, place zinc diethyldithiocarbamate (0.842 mmol), copper(II) acetate (1.58 mmol), and tin(II) acetylacetonate (0.846 mmol) in a 20 mL vial equipped with a stir bar . 2-Aminopyridine (1.0058 g) was added, followed by 5.05 mmol of (ethylthio)trimethylsilane and 0.814 mmol of sulfur. The reaction mixture was stirred at the first heating temperature of 105°C for ~40 hours. The reaction mixture was then stirred at a second heating temperature of 190°C for ~8 hours. In a similar manner as described above in Example 1, the treated glass slide was coated by drop coating to make Coated Substrate 2A, and dried at 170°C for ~0.5 hours.

[0097] This process was repeated except that 3-aminopyridine was used as solvent to prepare coated substrate 2B. XAS analysis of coated substrates 2A and 2B confirmed the presence of CZTS with low Cu / Zn for 2A and 2B (Cu / Zn=1.06 in kesterite for 2A and 1.06 in kesterite for 2B. Cu / Zn=1.10).

Embodiment 3

[0099]

[0100] Zinc methoxyethoxide (1.638 mmol), copper(I) acetate (3.263 mmol), di-n-butyltin sulfide (1.631 mmol) and 2-mercaptoethanol (6.885 mmol) were placed together in a 40 mL amber in vial. 4-tert-butylpyridine (1.857 g) was added, and the resulting mixture was stirred well. Then 1.634 mmol of elemental sulfur were added. The reaction mixture was stirred at room temperature for ~12 hours, then at 105 °C for ~40 hours. The reaction mixture was then stirred at 190°C for ~16 hours. According to the method of Example 1, SLG-coated substrate 3A was prepared by drop coating and dried at 250° C. for 0.5 hours.

[0101] This process was repeated, using 2-aminopyridine as solvent, and the reaction mixture was stirred at a second heating temperature of 170° C. for ~8 hours to produce coated substrate 3B. This process was repeated, using 4-tert-butylpyridine as solvent, and the reaction mixture was stirred at a second heating temperature of 160° C. for ~8 hours to produc...

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Abstract

This invention relates to processes for making kesterite compositions with atypical Cu:Zn:Sn:S ratios and / or kesterite compositions with unusually small coherent domain sizes. This invention also relates to these kesterite compositions and their use in preparing CZTS films.

Description

field of invention [0001] The present invention relates to methods for preparing kesterite compositions having atypical Cu:Zn:Sn:S ratios and / or kesterite compositions having unusually small coherent crystal domain sizes. The present invention also relates to these kesterite compositions and their use in the preparation of CZTS films. Background of the invention [0002] Crystalline multinary metal chalcogenide compositions containing only nontoxic and highly abundant elements are of particular interest in developing environmentally sustainable processes and devices. Copper tin sulfide (Cu 2 SnS 3 or "CTS") and copper zinc tin sulfide (Cu 2 ZnSnS 4 or "CZTS") are particularly useful examples of such materials and are of interest because of their potential applications as small bandgap semiconductors, as nonlinear materials, and as suitable candidates for photovoltaic cell materials. [0003] Thin film photovoltaic cells typically use semiconductors such as CdTe or coppe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/00C01G19/00C09D11/00C23C18/12H01L31/04
CPCH01L31/18C01B19/002C01G19/006C23C18/1204C23C18/1283Y02E10/50H01L31/0326C09D11/52
Inventor L.K.约翰逊H.D.罗森菲尔德D.R.拉杜
Owner EI DU PONT DE NEMOURS & CO
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