United States Patent 11» Horn Feja et al. [54] PROCESS AND APPARATUS FOR PRODUCING PHOSPHINE-CONTAINING GAS [75] Inventors: Franziskus Horn Feja, Santiago, Chiles ‘Christoph Reichmuth, Berlin, Germany [73] Assignee: Degesch de Chile Ltda, Santiago, Chile [+] Notice: ‘This patent is subject to texminal dis- claimer, [21] Appl. No.: 08/689,911 [22] Filed: Jun. 7, 1996 [30] Foreign Application Priority Data Jon, 7, 1995 [OB] United Kingdom osin495 [51] Int. cL? COUB 25/06 [2] U 282/372 [58] Field of Search 252872 [56] References Cited USS. PATENT DOCUMENTS 48144154 3/1989 Doermmann et US006027667A_ uy) Patent Number: 6,027,667 [45] Date of Patent: *Feb. 22, 2000 5,573,740 11/1996 Banks et al. FOREIGN PATENT DOCUMENTS 201807 6/1928, 472070 10/1937 796070 6/1937 2062602 12/197 2007775 5/1981 ‘9325075 12/1993, United Kingdom United Kingdom United Kingdom United Kingdom United Kingdom ‘WIPO Primary Examiner—Michael L. Shippen Attorney, Agent, or Firn—Pillsbury Madison & Suteo LLP 157) ABSTRACT ‘A process and apparatus is disclosed for generating a mix- ture of phosphine and diluent gas(es). A hydrolyzable metal phosphide, preferably magnesium phosphide, is released directly into liquid water under an atmosphere of gas inert to phosphine and in a free-flowing particulate form, composed ‘of loose metal phosphide particles. The generated mixture of phosphine and inert carrer gas, e:2, CO,, is used as such or is diluted into a gas mixing chamber with air to a concen- tration below the ignitability limit before being used in fumigation, Using argon as a cartier gas the phosphine ‘mixture is suitable for semiconductor doping. 47 Claims, 5 Drawing Sheets6,027,667 Sheet 1 of 5 Feb. 22, 2000 US. Patent6,027,667 Sheet 2 of 5 Feb. 22, 2000 US. Patent