C01G39/04

MOLYBDENUM OXYCHLORIDE OR TUNGSTEN OXYCHLORIDE AND PRODUCTION METHOD THEREOF
20210053839 · 2021-02-25 ·

A molybdenum oxychloride or a tungsten oxychloride, wherein the molybdenum oxychloride or the tungsten oxychloride has a moisture content of less than 1 wt %. A method of producing a molybdenum oxychloride or a tungsten oxychloride, wherein a molybdenum oxide or a tungsten oxide as a raw material is subject to dehydration treatment at 400 C. or higher and 800 C. or less, and the raw material that underwent dehydration treatment is thereafter reacted with a chlorine gas to synthesize a molybdenum oxychloride or a tungsten oxychloride. An object of the present invention is to provide a molybdenum oxychloride or a tungsten oxychloride having a low moisture content, as well as a production method thereof.

OXYHALIDE PRECURSORS

The invention provides a process for preparing molybdenum and tungsten oxyhalide compounds which are useful in the deposition of molybdenum and tungsten containing films on various surfaces of microelectronic devices. In the process of the invention, a molybdenum or tungsten trioxide is heated in either a solid state medium or in a melt-phase reaction comprising a eutectic blend comprising alkaline and/or alkaline earth metal salts. The molybdenum or tungsten oxyhalides thus formed may be isolated as a vapor and crystallized to provide highly pure precursor compounds such as MoO.sub.2Cl.sub.2.

OXYHALIDE PRECURSORS

The invention provides a process for preparing molybdenum and tungsten oxyhalide compounds which are useful in the deposition of molybdenum and tungsten containing films on various surfaces of microelectronic devices. In the process of the invention, a molybdenum or tungsten trioxide is heated in either a solid state medium or in a melt-phase reaction comprising a eutectic blend comprising alkaline and/or alkaline earth metal salts. The molybdenum or tungsten oxyhalides thus formed may be isolated as a vapor and crystallized to provide highly pure precursor compounds such as MoO.sub.2Cl.sub.2.

Production method and production apparatus for molybdenum hexafluoride

The present invention provides a method of producing high-purity molybdenum hexafluoride in good yield and a reaction apparatus therefor. The method of producing molybdenum hexafluoride in a production apparatus for molybdenum hexafluoride, which production apparatus includes a fixed bed that is for mounting metallic molybdenum and that extends inside a reactor from an upstream side to a downstream side of the reactor, a fluorine (F.sub.2) gas inlet provided on the upstream side of the reactor, and a reaction product gas outlet provided on the downstream side of the reactor, comprises bringing metallic molybdenum into contact with fluorine (F.sub.2) gas, where the fixed bed for mounting metallic molybdenum is tilted.

Production method and production apparatus for molybdenum hexafluoride

The present invention provides a method of producing high-purity molybdenum hexafluoride in good yield and a reaction apparatus therefor. The method of producing molybdenum hexafluoride in a production apparatus for molybdenum hexafluoride, which production apparatus includes a fixed bed that is for mounting metallic molybdenum and that extends inside a reactor from an upstream side to a downstream side of the reactor, a fluorine (F.sub.2) gas inlet provided on the upstream side of the reactor, and a reaction product gas outlet provided on the downstream side of the reactor, comprises bringing metallic molybdenum into contact with fluorine (F.sub.2) gas, where the fixed bed for mounting metallic molybdenum is tilted.

PRODUCTION OF MoO2Cl2

The invention relates to a method for producing MoO.sub.2Cl.sub.2 under inert conditions, comprising the steps of: (i) charging a reaction vessel with MoO.sub.2, (ii) reacting the MoO.sub.2 with supplied Cl.sub.2 in the reaction vessel at a first temperature T.sub.1 to give gaseous MoO.sub.2Cl.sub.2, (iii) transferring the gaseous MoO.sub.2Cl.sub.2 into a receiving vessel, (iv) resublimating the gaseous MoO.sub.2Cl.sub.2 in the receiving vessel to give solid MoO.sub.2Cl.sub.2 at a second temperature T.sub.2 that is lower than T.sub.1, and (v) recovering solid MoO.sub.2Cl.sub.2 with a purity determined by ICP-OES/MS of 99.9996 wt. % or more.

The invention also relates to high-purity MoO.sub.2Cl.sub.2, the use thereof, and electronic components.

PRODUCTION OF MoO2Cl2

The invention relates to a method for producing MoO.sub.2Cl.sub.2 under inert conditions, comprising the steps of: (i) charging a reaction vessel with MoO.sub.2, (ii) reacting the MoO.sub.2 with supplied Cl.sub.2 in the reaction vessel at a first temperature T.sub.1 to give gaseous MoO.sub.2Cl.sub.2, (iii) transferring the gaseous MoO.sub.2Cl.sub.2 into a receiving vessel, (iv) resublimating the gaseous MoO.sub.2Cl.sub.2 in the receiving vessel to give solid MoO.sub.2Cl.sub.2 at a second temperature T.sub.2 that is lower than T.sub.1, and (v) recovering solid MoO.sub.2Cl.sub.2 with a purity determined by ICP-OES/MS of 99.9996 wt. % or more.

The invention also relates to high-purity MoO.sub.2Cl.sub.2, the use thereof, and electronic components.

Oxyhalide precursors

The invention provides a process for preparing molybdenum and tungsten oxyhalide compounds which are useful in the deposition of molybdenum and tungsten containing films on various surfaces of microelectronic devices. In the process of the invention, a molybdenum or tungsten trioxide is heated in either a solid state medium or in a melt-phase reaction comprising a eutectic blend comprising alkaline and/or alkaline earth metal salts. The molybdenum or tungsten oxyhalides thus formed may be isolated as a vapor and crystallized to provide highly pure precursor compounds such as MoO.sub.2Cl.sub.2.

Oxyhalide precursors

The invention provides a process for preparing molybdenum and tungsten oxyhalide compounds which are useful in the deposition of molybdenum and tungsten containing films on various surfaces of microelectronic devices. In the process of the invention, a molybdenum or tungsten trioxide is heated in either a solid state medium or in a melt-phase reaction comprising a eutectic blend comprising alkaline and/or alkaline earth metal salts. The molybdenum or tungsten oxyhalides thus formed may be isolated as a vapor and crystallized to provide highly pure precursor compounds such as MoO.sub.2Cl.sub.2.

OXHALIDE PRECURSORS

The invention provides a process for preparing molybdenum and tungsten oxyhalide compounds which are useful in the deposition of molybdenum and tungsten containing films on various surfaces of microelectronic devices. In the process of the invention, a molybdenum or tungsten trioxide is heated in either a solid state medium or in a melt-phase reaction comprising a eutectic blend comprising alkaline and/or alkaline earth metal salts. The molybdenum or tungsten oxyhalides thus formed may be isolated as a vapor and crystallized to provide highly pure precursor compounds such as MoO.sub.2Cl.sub.2.