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A Concise History of Vacuum Coating Technnology SVC Topics SVCSVC TopicsTopics Donald M. Mattox, Technical Director • Society of Vacuum Coaters 71 Pinon Hill Place N.E. • Albuquerque, NM 87122 505/856-7188 • FAX: 505/856-6716 • www.svc.org A Concise History Of Vacuum Coating Technnology Part I: Prior to WWII (1940) Before the mid-1930s, many tech- niques for vaporizing material and depositing coatings in vacuum had been demonstrated; however, they remained mostly laboratory curiosi- ties. This was mainly because of the lack of good vacuum materials and systems. In the mid-1930s, improve- ments in materials, techniques and equipment led to the development of commercial applications of vacuum deposition for zinc-metallized paper for paper capacitors for the electron- ics industry, reflector coatings for mirrors and lighting and antireflection coatings for optics. The advent of World War II led to a dramatic increase in the use of vacuum coat- Apparatus for the production of mirrors by (a) Apparatus for the production of mirrors by (b) cathode sputtering. “This method for the evaporation of metal. “This method of deposition ings. preparation of reflecting surfaces is particularly has not been widely tested, and its possibilities The deposition of coatings in a useful as a process for half-silvering and for are, therefore, little known, but it would seem to vacuum environment was known for a depositing metals other than silver. ... For joint be especially valuable for small work where films long time before the process was used grease, a special solution of crude rubber and of any volatile substance are required. ... The commercially. Vacuum deposition of lard was made. ... A 10,000-volt transformer glass gube may be made entire, then cracked off furnishes the current; and it is advisable, although at (h) and subsequent sealings be accomplished a coating consists of a source of the not absolutely necessary, to rectify the current.” with sealing wax.” material to be deposited, transport of Figures and quotes are from the Bureau of Standards Circular #389, “The Making of Mirrors the material through a low-pressure by the Deposition of Metal on Glass,” January 1931. gaseous (or plasma) environment and condensation on a substrate. In some ization) or from a combination of deposition by thermal evaporation cases, the depositing material reacts processes (hybrid deposition process). (from a crucible) by Nahrwold (1887) with the gaseous environment, or a In PVD, the principal vaporization and Pohl and Pringsheim (1912). co-deposited material, to form a techniques are thermal evaporation/ Vacuum pyrolysis of hydrocarbon coating of a chemical compound, such sublimation, sputtering and arc vapors to form carbon films was as a nitride or carbide (reactive vaporization. reported by Sawyer and Mann (1880), deposition). The source of the Arc vaporization in vacuum was and the hydrogen reduction of WCl4 material can be a solid or liquid first reported by Hare (1939). Grove to form tungsten films was reported surface that is vaporized (physical (1852) and Pulker (1858) first by de Lodyguine (1897). vapor deposition, or PVD), from a reported vaporization by sputtering. To deposit a solid film in a vacuum chemical vapor precursor (subatmo- Electric discharge vaporization of by PVD processes, it is necessary to spheric chemical vapor deposition, or wires was first reported by Faraday reduce the gas pressure to the extent SA-CVD), from a chemical monomer (1857). Plasma polymerization of that collisions in the gas phase do not generally in plasma (plasma polymer- organic monomers was reported by produce gas-phase nucleation and _____________ deWilde (1874) and Thenard (1874). “soot,” rather than a solid film. This Columnist’s Note: This is Part 1 of a Sputter deposition of films was requires a pressure of less than about three-part series. reported by Wright (1877) and film 0.0001 atmospheres. That vacuum March 2000 59 could be attained with some early system—only an optical baffle depositing film material. After about “mercury piston” pumps. By 1880, between the vacuum pump and the 1930, with the advent of better seals, Edison had achieved a “good” processing chamber. This made for a better vacuum pumps and evaporation vacuum of about 10-6 atmospheres, as slow cycle time, because the oil from tungsten filaments (Ritschl, measured by a McLeod vacuum diffusion pump had to heat up and 1928; Strong, 1929), most films were gauge (McLeod, 1874) using a cool down on each cycle. deposited by thermal evaporation. combination of Geissler (1858) and A major obstacle to producing Ruhle described the use of an electron Sprengel (1865) glass mercury piston vacuum-deposited films was the lack beam for thermal evaporation in 1940, pumps, chamber heating (“flaming”) of accessibility to the vacuum but e-beam evaporation for vacuum and cold traps. This level of vacuum chamber. Greases, waxes and oiled coating did not become commonplace was necessary to prevent oxygen from leather were common vacuum until the early 1950s. In 1938, Strong burning out the carbon filaments used sealants but, because of their high published his book, Procedures in in the production of the first light vapor pressures, did not allow heating Experimental Physics (Prentice-Hall), bulbs (Edison, 1879). the vacuum chamber enough to which discussed many aspects of Another requirement is to reduce achieve the good vacuum necessary vacuum technology and film deposi- the gaseous contaminant level in the for thermal evaporation in a demount- tion of that period. deposition environment to a level that able system. The figure shows a Deposition of chemically reactive is acceptable. Contamination can sputtering chamber and a vacuum materials in a partial pressure of a affect both the deposited film material evaporation chamber as published in reactive gas can produce films of a and the material in the vaporization the Bureau of Standards Circular compound material (reactive deposi- source. Before 1940, the principal #389, “The Making of Mirrors by the tion), but early films formed this way non-fluid vacuum gauges were the Deposition of Metal on Glass” were of poor quality. Reactive Piriani (Piriani, 1906), thermocouple (January 1931), along with some evaporation was first reported by (Voege, 1906), bourdon (Lorenz, excerpts describing the processes. Soddy in 1907, and reactive sputter 1917) and cold cathode ionization Low-vapor-pressure greases and deposition was studied by Berraz in (Penning, 1937) gauges. The concept waxes were introduced by Burch in 1933. Also in 1933, Overbeck of the viscosity (molecular drag) 1929 (Apiezon waxes and greases), advanced the idea that oxide films gauge (Hogg, 1906) and capacitance but it was not until the mid-1930s that could be deposited for optical manometer gauge (Olsen & Hirst, fairly reliable, nonpermanent (break- coatings; numerous papers on the 1929) were known, but not well able) “bakeable” vacuum seals came subject followed. developed. into use and allowed good vacuums In 1930, Pfund evaporated metals In the best early vacuum systems, and repetitive easy access to the into a poor vacuum to form very fine the glass vacuum chamber was fused vacuum chamber. One of these was particles by gas phase nucleation (gas to the glass vacuum pump and fusion- the lead-wire “corner seal” described evaporation). A layer of ultrafine sealed (“tipped off”) when the desired by Strong in 1938. Neoprene (“artifi- particles of gold (black gold “smoke”) vacuum was attained. This procedure cial”) rubber was invented by DuPont is still used as a very efficient infrared- was acceptable for the production of in 1933, and molded seals of this radiation absorber. This technique is light bulbs and early studies involving material began to be used in the late used today to form “nanoparticles” of vacuum and plasmas, such as the gas- 1930s. a variety of materials. discharge tubes (Crookes, 1879), X- Before the 1930s, sputter deposi- After the 1930s, the primary ray tubes (Rontgen, 1895), discovery tion was the most widely used disadvantage of sputtering was that of the electron (Thompson, 1898) and vacuum coating process. Edison, for most materials of interest could be the triode electron tube (DeForest, example, patented a process for deposited by thermal evaporation 1906). The procedure was not sputter deposition of films on the faster and cheaper. The fundamental amendable to depositing films on masters for wax phonograph cylinders phenomena of sputtering was studied substrates in any commercial quantity. in 1904. Sputtering could be used for by Guntherschutzer in the 1920s and The use of cold traps to keep mercury vacuum coating because it is a low- 1930s, who established that the from the processing chamber was temperature vaporization process that vaporization by sputtering was non- improved by the use of liquefied air does not require a very good vacuum thermal process caused by momentum (1885) and the development of a for the deposition of non-reactive transfer from high-energy bombarding means for its storage in a vacuum- materials. The low temperature ions. An effect that later had a major insulated vessel (Dewar, 1892). The avoided vaporization of oils, greases impact on sputtering was the use of development of the mercury diffusion and waxes used for sealing and magnetic and electric fields to confine pump (Gaede, 1913; Langmuir, 1916) minimized reaction of the deposited electrons, which was reported by allowed good vacuums to be attained film material with gaseous contami- Penning in 1936. In the late 1960s and more easily than with the mercury nants. early 1970s, the “Penning effect” was piston pumps. The replacement of Thermal evaporation, on the other used to enhance the ionization in the mercury by refined low-vapor- hand, is a high-temperature process low-pressure plasmas utilized for pressure hydrocarbon oils (Burch, where the radiant heat from the sputtering (magnetron sputtering). 1928; Hickman, 1929) in the diffusion vaporization source heats the chamber Resurgence of sputter deposition pumps allowed the elimination of cold and associated seals.
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