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Silyl phosphine compound, method for producing silyl phosphine compound and method for forming InP quantum dot

A technology of silylphosphine and manufacturing method, which is applied in the direction of silicon organic compounds, phosphorus compounds, phosphorus organic compounds, etc., and can solve the problems of cadmium toxicity and high environmental burden

Pending Publication Date: 2020-10-30
NIPPON CHECMICAL IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, cadmium has high toxicity and environmental burden, so the development of cadmium-free quantum dots is expected

Method used

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  • Silyl phosphine compound, method for producing silyl phosphine compound and method for forming InP quantum dot
  • Silyl phosphine compound, method for producing silyl phosphine compound and method for forming InP quantum dot
  • Silyl phosphine compound, method for producing silyl phosphine compound and method for forming InP quantum dot

Examples

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Embodiment

[0143] Hereinafter, the present invention will be described in more detail with examples, but the present invention is not limited to these examples. In addition, in the following, as each solvent, a solvent whose moisture content is reduced to 10 ppm or less on a mass basis is used. The moisture content was measured using a Karl Fischer moisture meter (MKC610 manufactured by Kyoto Electronics).

[0144]

[0145] After adding 189.8 kg of toluene to the reaction vessel, 82 kg of triethylamine and 149.5 kg of trimethylsilyl trifluoromethanesulfonate were added, the inside of the reaction vessel was replaced with nitrogen, and the liquid temperature was adjusted to 30°C.

[0146] A stainless steel pressure column with an inner diameter of 25 cm and a length of 2 m was filled with 8.5 kg of granular activated carbon (manufactured by TSURUMI COAL CO., LTD.) to prepare an adsorption tower. 7.5 kg of crude phosphine gas (manufactured by Nippon Chemical Industry Co., Ltd.) with an arsenic...

Embodiment 2

[0188] (Synthesis of InP quantum dots)

[0189] 0.375 mmol of indium myristate was added to 17.8 g of 1-octadecene, and the mixture was heated to 120° C. while stirring under reduced pressure, and degassed for 90 minutes. After degassing, it was cooled to 70°C to obtain a 1-octadecene solution of indium myristate. In addition, 0.25 mmol of tris(trimethylsilyl)phosphine (TMSP) obtained in Example 1 was added to 0.6 g of 1-octadecene to obtain a 1-octadecene solution of TMSP. After heating the obtained 1-octadecene solution of TMSP to 70°C, it was added to the 1-octadecene solution of indium myristate, and the temperature was raised to 300°C while stirring, and then kept for 2 minutes to obtain Red liquid of InP quantum dots.

[0190] (Synthesis of InP / ZnSe / ZnS quantum dots)

[0191] Add 4.5mmol of zinc myristate to 18.6g of 1-octadecene, heat to 120°C while stirring under reduced pressure, and degas for 90 minutes to obtain a 1-octadecene solution of zinc myristate . In the obtai...

Embodiment 3

[0199] (Synthesis of InZnP quantum dots)

[0200] 2.4 mmol of indium myristate and 1.6 mmol of zinc myristate were added to 63.4 g of 1-octadecene, heated to 110° C. while stirring under reduced pressure, and degassed for 90 minutes. After degassing, the temperature was raised to 300°C to obtain a 1-octadecene solution of indium myristate and zinc myristate. In addition, 1.0 mmol of tris(trimethylsilyl)phosphine (TMSP) obtained in Example 1 was added to 2.25 g of 1-octadecene to obtain a 1-octadecene solution of TMSP. The obtained 1-octadecene solution (room temperature) of TMSP was added to the 1-octadecene solution of indium myristate and zinc myristate, and the mixture was kept at 300°C for 30 minutes while stirring to obtain InZnP Crimson liquid with quantum dots.

[0201] (Synthesis of InZnP / ZnSe / ZnS quantum dots)

[0202] Bring the liquid containing InZnP quantum dots to 220°C, add 22.0 mmol of trioctyl phosphine selenide, and heat to 260°C. In addition, 12.0 mmol of zinc m...

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Abstract

A silyl phosphine compound according to the present invention is represented by formula (1) and has an arsenic content of 1 ppm or less. A method according to the present invention for producing the silyl phosphine compound comprises: mixing a basic compound, a silylating agent and phosphine to give a solution containing a silyl phosphine compound; removing the solvent from the solution to give aliquid concentrate containing the silyl phosphine compound; and then distilling the liquid concentrate, wherein the arsenic content of the phosphine is regulated to 1 ppm by volume or less in terms ofarsine. In the method according to the present invention for forming an InP quantum dot, the silyl phosphine compound that is represented by formula (1) (wherein R is as defined in the description) and has an arsenic content of 1 ppm by mass or less is used as a phosphorus source.

Description

Technical field [0001] The present invention relates to a method for producing a silylphosphine compound that can be effectively used as a raw material for the phosphorus component of indium phosphorus quantum dots. Background technique [0002] In recent years, as a luminescent material, the development of quantum dots has gradually progressed. As a representative quantum dot, the development of cadmium-based quantum dots such as CdSe, CdTe, CdS, etc. has gradually progressed due to its excellent optical properties. However, cadmium has a high toxicity and environmental burden, so the development of cadmium-free quantum dots is expected. [0003] As one of the cadmium-free quantum dots, indium phosphorus (InP) can be cited. In the production of indium phosphorus, a silylphosphine compound such as tris(trimethylsilyl)phosphine is often used as a raw material for its phosphorus component. Silyl phosphine compounds such as tris (trimethylsilyl) phosphine can be used in a solid sta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00C01B25/08H01L29/06C07F7/08C07F9/50
CPCC01B25/08H01L29/06C09K11/70C01B25/087C07F9/062C07F19/00C07F9/5004C07F7/0805C07F7/0834C09K11/025C09K11/883C09K11/565C07F9/06C07F7/08C07F9/5009
Inventor 田久保洋介田村健中对一博
Owner NIPPON CHECMICAL IND CO LTD
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