Entegris, Inc.

USA As Represented by Secretary of the Navy

Robert Wright, Jr

Thomas H Baum

Bryan Clark Hendrix

David M Ermert

Scott L Battle

Philip S H Chen

David James Eldridge

John N Gregg

David Walter Peters

John M Cleary

Han Wang

Shawn D Nguyen

Michael W Geis

John H Coates

James E Butler

Shuang Meng

James Woeckener

Yuqi Li

Donald D Flechtner

Described are vapor deposition methods for depositing metal films or layers onto a substrate, e.g., wherein the metal is molybdenum or tungsten; the methods involve vapor deposition of a metal layer onto a substrate from a metal-containing precursor in the presence of reducing gas (e.g., hydrogen) and a nitrogen-containing reducing compound.

Methods for depositing a tungsten or molybdenum layer in the presence of a reducing co-reactant

The invention provides a facile process for preparing various Group VI precursor compounds useful in the vapor deposition of such Group VI metals onto solid substrates, especially microelectronic semiconductor device substrates. The process provides an effective means to obtain such volatile materials, which can then be sources of molybdenum, chromium, or tungsten-containing materials to be deposited on such substrates. Additionally, the invention provides a method for vapor deposition of such compounds onto microelectronic device substrates.

Group VI precursor compounds

Described are vapor deposition methods for depositing metal films or layers onto a substrate, wherein the metal is molybdenum or tungsten; the methods involve organometallic precursor compounds that contain the metal and one or more carbon-containing ligands, and include depositing a metal layer formed from the metal of the precursor, onto a substrate, followed by introducing oxidizer to the formed metal layer.

Methods for depositing tungsten or molybdenum films

Provided is a process for the rapid deposition of highly conformal molybdenum- or tungsten-containing films onto microelectronic device substrates under vapor deposition conditions. In the practice of the invention, a first nucleation step is conducted, while utilizing a generally lower concentration of metal precursor than would ordinarily be utilized in the reaction zone. This utilization of lower metal precursor concentrations can be achieved by way of regulating the temperature of the ampoule (housing the precursor), the concentration of the precursor, pressure in the reaction zone, and the duration of the pulse. In this fashion, a generally lower concentration is utilized to form a nucleation layer of greater than or equal to about 3 Å, or up to about 9, 15, or 25 Å, at which time, the conditions for introducing the precursor are advantageously changed and the concentration of the precursor in the reaction zone is increased for the purpose of bulk deposition.

Deposition process for molybdenum or tungsten materials

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 MoOCl.

Oxyhalide precursors

A chemical delivery system includes a bulk container, a run/refill chamber, a first conduit and a second conduit. The bulk container stores a precursor. The run/refill chamber includes a plurality of spaced tubes having a plurality of surfaces for receiving the precursor in vapor form and storing the precursor in solid form. The first conduit connects the bulk container to the run/refill chamber for transporting the precursor from the bulk container to the run/refill chamber in vapor form. The second conduit connects the run/refill chamber to a deposition chamber for transporting the precursor from the run/refill chamber to the deposition chamber in vapor form.

Chemical delivery system and method of operating the chemical delivery system

A methodology for (a) the etching of films of AlO, HfO, ZrO, W, Mo, Co, Ru, SiN, or TiN, or (b) the deposition of tungsten onto the surface of a film chosen from AlO, HfO, ZrO, W, Mo, Co, Ru, Ir, SiN, TiN, TaN, WN, and SiO, or (c) the selective deposition of tungsten onto metallic substrates, such as W, Mo, Co, Ru, Ir and Cu, but not metal nitrides or dielectric oxide films, which comprises exposing said films to WOClin the presence of a reducing gas under process conditions.

Method for etching or deposition

Described are vapor deposition methods for depositing molybdenum materials onto a substrate by the use of bis(alkyl-arene) molybdenum, also referred to herein as (alkyl-arene)Mo, for example bis(ethyl-benzene) molybdenum ((EtBz)Mo), as a precursor for such deposition, as well as structures that contain the deposited material.

Vapor deposition of molybdenum using a bis(alkyl-arene) molybdenum precursor

A solid delivery precursor is described, which is useful for volatilization to generate precursor vapor for a vapor deposition process. The solid delivery precursor comprises solid bodies of compacted particulate precursor, e.g., in a form such as pellets, platelets, tablets, beads, discs, or monoliths. When utilized in a vapor deposition process such as chemical vapor deposition, pulsed chemical vapor deposition, or atomic layer deposition, the solid delivery precursor in the form of solid bodies of compacted particulate precursor provide substantially increased flux of precursor vapor when subjected to volatilization conditions, in relation to the particulate precursor. As a result, vapor deposition process operation can be carried out in shorter periods of time, thereby achieving increased manufacturing rates of products such as semiconductor products, flat-panel displays, solar panels, LEDs, optical coatings, and the like.

Cold sintering of solid precursors

A solid source material is described for forming a tungsten-containing film. The solid source material is tungsten hexacarbonyl, wherein content of molybdenum is less than 1000 ppm. Such solid source material may be formed by a process including provision of particulate tungsten hexacarbonyl raw material of particles of size less than 5 mm, wherein particles of size greater than 1.4 mm are less than 15% of the particles, and wherein content of molybdenum is less than 1000 ppm, and sintering the particulate tungsten hexacarbonyl raw material at temperature below 100&#xb0; C. to produce the solid source material as a sintered solid.

High-purity tungsten hexacarbonyl for solid source delivery

A multipass cell assembly for monitoring of fluid is described, as well as fluid processing systems utilizing same, and associated methods of use of such multipass cell assembly for fluid monitoring. The multipass cell assembly is usefully employed in fluid processing operations such as monitoring of vapor deposition process reactants, e.g., reactants used for vapor deposition metallization of tungsten from a tungsten carbonyl precursor.

Growing community of inventors

Newtown, CT, United States of America

Robert Wright, Jr