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HHHHHH US005082696A United States Patent (19) 11 Patent Number: 5,082,696 Sharp (45) Date of Patent: Jan

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HHHHHH US005082696A United States Patent (19) 11 Patent Number: 5,082,696 Sharp (45) Date of Patent: Jan HHHHHH US005082696A United States Patent (19) 11 Patent Number: 5,082,696 Sharp (45) Date of Patent: Jan. 21, 1992 54) METHOD OF FORMING 4,217,374 8/1980 Ovshinsky et al. .............. 427/248.1 SEMICONDUCTING AMORPHOUS 4,466,992 8/1984 Dreiling ....... ... ... 427/255. SILICON FILMS FROM THE THERMAL 4,469,045 9/1984 Chesworth .... ... 427/255.5 4,485,121 1/1984 Matsumura ..., ... 427/39 DECOMPOSITION OF DIHALOSILANES 4,634,605 1/1987 Wiesmann ........................ 427/255.1 (75) Inventor: Kenneth G. Sharp, Midland, Mich. OTHER PUBLICATIONS (73) Assignee: Dow Corning Corporation, Midland, Auguelli and Murri, Mter, Chem. and Phys. (Switzer Mich. land) 9, 301-5 (1983). (21) Appl. No.: 140,191 Everysteyn, Chemical-Reaction Engineering in the Filed: Dec. 31, 1987 Semi-Conductor Industry, Philips Res. Repts. 29, 22 45-46, 1974. Scott et al., Kinetics and Mechanism of Amorphous Related U.S. Application Data Hydrogenated Silicon Growth by Homogeneous (63) Continuation-in-part of Ser. No. 914,898, Oct. 3, 1986, Chemical Vapor Deposition, Appl., Phys., Lett. 39 (1) abandoned. Jul. 1981. (51) Int. Cl. ....................... C23C 16/00; C23C 16/46 Primary Examiner-Shrive Beck (52) U.S. Cl. .................................... 427/255; 427/162; Attorney, Agent, or Firm-James E. Bittell; Roger E. 427/167; 427/255.1; 427/255.2 Gobrogge (58) Field of Search .................. 427/248. 1, 255.1, 255, 427/162, 167, 255.2; 428/446, 450 (57) ABSTRACT 56 References Cited The invention relates to the chemical vapor deposition of dihalogenated silanes to form stable, abrasion resis U.S. PATENT DOCUMENTS tant, photoconductive, dopable semiconductor anor 2,148,328 5/1985 Hirooka et al. .... ... 427/248.1 phous films on substrates. Additional hydrogen and 2,788,280 4/1957 Rust et al. .......... ... 427/248. plasma discharge conditions are not necessary to prac 3,809,571 5/1974 Berlat ......... ... 427/248. 4,064,521 12/1976 Carlson ... ... 427/255.1 tice the invention. 4,196,438 4/980 Carlson ................................. 427/39 4,217,148 8/1980 Carlson ................................. 427/39 17 Claims, No Drawings 5,082,696 1 2 The obvious disadvantage of such prior art, one which METHOD OF FORMING SEMICONEOUCTING clearly distinguishes it from the instant invention, is the AMORPHOUS SILICON FILMS FROM THE necessity of having two materials to decompose. THERMAL DECOMPOSITION OF Hirooka, et al. requires the second stream as the source DHALOSILANES of hydrogen to facilitate the reduction of the halosilane to the amorphous silicon. The instant invention, how This application is a continuation-in-part of copend ever, has sufficient hydrogen in the single component ing application Ser. No. 914,898 filed on Oct. 3, 1986, dihalomonosilane to produce the desired amorphous now abandoned. silicon film. Several of the molecular precursors O claimed by Hirooka, et al., such as (SiH2)3 or (SiX2)3, BACKGROUND OF THE INVENTION where X=F or Cl have either not been reported as The present invention relates to the discovery that being prepared elsewhere in the literature or have pyrolysis of certain dihalogenated monosilanes or mix proved exceedingly difficult to synthesize. Hirooka, et tures of dihalogenated monosilanes can result in the al., does not teach the synthesis of these elusive mole formation of a highly stable, highly abrasion resistant, 15 cules. photoconductive, dopable semiconductor film on a United Kingdom Patent number 2,156,385, issued substrate. Oct. 9, 1985 to Tanaka et al., teaches the deposition of a Amorphous polymeric materials of silicon and hydro silicon film on a heated substrate from a reactant gen (hereafter referred to as a-SiH) have emerged as a fluorosilane gas in the plasma state. However, Tanaka et new class of semiconductors in recent years. Such mate 20 al. does not teach the use of chemical vapor deposition rials are described, for example, in D. Carlson, U.S. Pat. of dihalosilanes to form amorphous silicon-containing No. 4,064,521, issued on Dec. 20, 1976. The materials films. are generated as thin films from the decomposition of Thus the instant invention is distinguished from prior silane (SiH4) in electrical discharges or, less frequently, art utilizing chemical vapor deposition of disilanes, from the thermal decomposition of silane or higher 25 polysilanes, and reduction systems requiring dual hydrogen-containing silanes (e.g., Si2H6, Si3H8, etc.) as streams of starting materials. The instant invention is described in a PCT patent application by A. MacDiar also distinguished from the prior art utilizing plasma mid and Z. Kiss published as International Publication deposition systems, No. WO 82/03069 dated Sept. 16, 1982. SUMMARY OF THE INVENTION When it is desirable to include additional elemental 30 constituents in the amorphous films, co-reactants such The present invention relates to the formation of as phosphine (PH3) or diborane (B2H6) are added to the amorphous silicon films prepared from the thermal starting materials. When fluorine is to be incorporated decomposition, often referred to as chemical vapor into an amorphous film, tetrafluorosilane (SiF4) is most deposition (CVD), of dihalosilanes. By "dihalosilane" commonly added to the reactant mixture. This is de 35 herein is meant a monosilane compound in which the scribed for example in U.S. Pat. No. 4,217,374 granted silicon aton has bonded to it two halogen atoms and to Ovshinsky and Izu on Aug. 12, 1980. Similarly, chlo two hydrogen atoms. The term "amorphous' is herein rine atoms can be incorporated into films via decompo construed to include both noncrystalline and microcrys sition of mixtures of silicon tetrachloride (SiCl4) and talline materials, in which the crystallites are less than silane or hydrogen (see, for example, V. Augelli and R. 50 Angstrons in dimension, and are not contiguous so Murri, Mater. Chem. and Phys. (Switzerland) 9, 301-5 as to form well defined grain boundaries. The films are (1983)). formed from decomposition of vapor phase A disadvantage to the use of silane, disilanes or dihalomonosilanes, X2SiH2, at elevated temperatures. polysilanes (SinH2n-2) as a starting material for genera No additional source of hydrogen is needed in the in tion of a-SiH relates to the high explosion hazard of 45 stant invention nor is the use of electric discharges silane/air mixtures. An operational consequence of this (plasma) necessary. The use of dihalosilane as source explosion hazard is the frequent use of inert carrier gas for the CVD method provides an important purifi gases as diluents in these systems. Both discharge cation capability over that of disilane (or higher molec (plasma) and chemical vapor deposition (CVD) routes ular weight) starting materials. Siloxane impurities in to a-SiH from silane also have disadvantageous features. 50 the disilane (and higher) source gases of the prior art Conventional discharge systems require relatively so can introduce unacceptably high amounts of oxygen phisticated and expensive equipment to remove the into the film being deposited. Siloxane impurities are reaction by-products. Silane-based CVD systems, while easily removed from dihalomonosilanes. It should also simple, suffer from a tendency to undergo vapor nucle be noted that tetrahalomonosilanes such as tetrachloro ation unless the pressure is very low. This behavior 55 or tetrafluorosilane and the corresponding trihalosilanes restricts the range of permissible operating conditions cannot be employed as starting materials in the decom for such thermal decompositions. position to provide satisfactory films according to the United Kingdom Patent No. 2,148,328, issued to M. invention. The instant invention also simplifies the feed Hirooka, et al., on May 30, 1985, teaches the decompo process of the material to be decomposed by reducing sition of various silanes, including halosilanes (SiX4), the number of reactants from two to one since an addi cyclic polymeric halosilanes (Six2)n, where n is greater tional source of hydrogen is not required. The hydro than or equal to 3, di- and polysilanes such as gen initially on the dihalosilane results in silicon-hydro SiHX2 and SinH2X2n. These materials are decom gen bonds in the film, said silicon-hydrogen bonds being posed via electric discharge, photolysis, high tempera known in the art to be associated with a lowering of the ture, or catalytically and mixed with a requisite second 65 defect density in the amorphous silicon film. stream consisting of a vapor phase material selected The instant invention also relates to a method of from the group consisting of H2. SiH4. SiH3Br, or SiH3I forming amorphous polymeric silicon-containing films wherein the second stream has also been decomposed. on a substrate which method comprises decomposing a 5,082,696 3 4. dihalosilane or mixture of dihalosilanes in the vapor poses and forms a silicon film on the substrate. Then the phase wherein the halogens of the dihalosilane or mix reaction by-products, trihalosilane and hydrogen (and ture of dihalosilanes are independently chosen from the any unreacted starting material if present), may conve group consisting of fluorine, chlorine, bromine, and niently be removed by evacuation after the deposition iodine, at a temperature between 400 degrees and 600 chamber has been reattached to the vacuum line. The C. in a reaction chamber containing a substrate which is substrate, onto which the decomposed dihalosilane thermally and chemically stable at the decomposition starting material has deposited an amorphous silicon temperature in the atmosphere of the reaction chamber, film, is then removed. By this method, difluorosilane whereby said films are formed on said substrate. A and dichlorosilane have been thermally decomposed in preferred temperature range for the thermal decomposi 10 the vapor phase to deposit amorphous silicon films on tion of the instant invention is between 450 and 570 C. various substrates. The resulting coatings are reflective, The instant invention features the further advantage air-stable, abrasion resistant, moisture resistant, photo that the dihalomonosilanes utilized are not susceptible conductive, semiconductive amorphous silicon-contain to vapor nucleation at higher pressures.
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