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(12) United States Patent (10) Patent No.: US 6,482,476 B1 Liu (45) Date of Patent: Nov USOO6482476B1 (12) United States Patent (10) Patent No.: US 6,482,476 B1 Liu (45) Date of Patent: Nov. 19, 2002 (54) LOW TEMPERATURE PLASMA ENHANCED 5,876,808 A * 3/1999 Hall et al. CVD CERAMIC COATING PROCESS FOR 6,110,571. A * 8/2000 Yaginuma et al. METAL, ALLOY AND CERAMIC MATERALS FOREIGN PATENT DOCUMENTS (75) Inventor: Shengzhong Frank Liu, 6084 Pond JP O7-216548 * 8/1995 plway, Mechanicsville, VA (US) OTHER PUBLICATIONS (73) Assignee: Shengzhong Frank Liu, Musher et al., J. Mater. Res., vol. 11, No. 4, Apr., 1996, pp. Mechanicsville, VA (US) 989-1OO1. (*) Notice: Subject to any disclaimer, the term of this * cited by examiner patent is extended or adjusted under 35 U.S.C. 154(b) by 0 days. Primary Examiner Timothy Meeks (21) Appl. No.: 09/465,405 (57) ABSTRACT (22) Filed: Dec. 16, 1999 A low temperature, high growth rate plasma enhanced O O chemical vapor deposition proceSS is demonstrated for Related U.S. Application Data ceramic coatings on metal, alloy and ceramic Substrates. The deposition process is carried out at low temperatures (<350 (63) Continuation-in-part of application No. 08/947.528, filed on degC.) to prevent the bulk Substrate properties from being Oct. 6, 1997, now abandoned. adversely affected. The Substrates are treated with gas Sur (51) Int. Cl. ................................................ C23C 16/30 face hardening processes before deposition. Bonding (52) U.S. Cl. ....................... 427,1535; 427/576; 427/577; strength (adhesion) between the coating and the Substrate is 427/585; 427/255.18; 427/255.31; 427/255.38; improved by combining Surface heat treating processes with 427/255.394 the coating processes. Hard ceramic-Solid lubricant compos (58) Field of Search ................................. 427/535, 576, ite coatings are used for fuel injector components, hydraulic 427/577, 585,255.394, 255.31, 255.38, valve components, and other wear parts. Metal-releasing 255.18 agents are used to improve deposition efficiency. Electron cyclotron resonance mechanism and electromagnetic radia (56) References Cited tion are used to improve bonding Strength, growth rate, coating uniformity, film Smoothness and other film qualities. U.S. PATENT DOCUMENTS 5,707,705 A * 1/1998 Nelson et al. 9 Claims, 5 Drawing Sheets 05 109 N O O)4 N. -/ 101 107 108 102 103 Power supply2. and 120 control U.S. Patent Nov. 19, 2002 Sheet 1 of 5 US 6,482,476 B1 105 120 Power supply and control U.S. Patent Nov. 19, 2002 Sheet 2 of 5 US 6,482,476 B1 Figure 2 Mixed gases Cathode rod -- A node - Substrate U.S. Patent Nov. 19, 2002 Sheet 3 of 5 US 6,482,476 B1 Figure Mixed gases l Magietron Pl Sila gas distribution ring Substrate holder Substrates U.S. Patent Nov. 19, 2002 Sheet 4 of 5 US 6,482,476 B1 Figure 4 Mixed gases powder feeder l - Plasma gas distribution ring & is: Electrode 3. - Substrate holder Substrate s: power Supply U.S. Patent Nov. 19, 2002 Sheet 5 of 5 US 6,482,476 B1 Figure S Mixed gases radiation source gas distribution ring Substrates Substrate holder US 6,482.476 B1 1 2 LOW TEMPERATURE PLASMA ENHANCED nitrogen are dissociated into nitrogen atoms. The highly CVD CERAMIC COATING PROCESS FOR energetic and active nitrogen atoms reacts with metal Sur METAL, ALLOY AND CERAMIC face and diffused into the Subsurface to form metal-nitrides. MATERALS If hydrocarbon is also introduced along with nitrogen and/or ammonia, the process is then called carbonitriding or CROSS-REFERENCE TO RELATED nitrocarburizing. In the like manner, Surface carburizing is APPLICATION(S) performed with hydrocarbon containing gases. This is a continuation-in-part of commonly-owned, The other method uses liquid bath-actually a molten copending U.S. patent application Ser. No. 08/947,528, filed nitrogen-containing Salt bath. The molten Salt reacts with the Oct. 6, 1997 now abandoned. metal Surface to form nitrides, carbides, and oxides. These nitriding, carburizing and carbonitriding processes BACKGROUND OF THE INVENTION may form up to millimeter deep nitride, carbide material Thanks to their Superior mechanical properties Such as over extended period of time. hardness, low coefficient of friction, thermal Stability at high 15 HEAT TREATMENT OF METAL AND ALLOY temperature, oxidation resistance, inertneSS to most common MATERIALS chemicals, and electrical and optical properties, ceramic materials are technologically important materials for many In general, heat treatment refers to a defined process applications, especially for high temperature, high power, which heats and cools a Solid metal or alloy in a controlled electronic barrier coatings, and cutting tool applications. For manner in order to improve Specific properties, Such as example, tungsten carbide (WC) including WC-Co alloys, hardness, Strength, ductility, magnetic Susceptibility, Silicon nitride, aluminum oxide, Silicon oxide, titanium toughness, machinability, fabricability, and even corrosion nitride, and titanium carbide are all very popular materials in resistance. According to this definition, heat treating has the market, particularly in machining business. long been practiced since ancient metalsmith or blackSmith 25 made bronze tools and iron-based Swords. Metals are still AS used herein, a "cerarnics material” includes nitrides, heat treated today, for the same reasons as ancient dayS oxides, borides, Sulfides, carbides, Suicides, carbon, hydro namely, to enhance or maximize mechanical properties of genated carbon materials and the like. the materials. Optimizing hardness, Strength, and other For example, titanium nitride has been exceptionally mechanical characteristics by heat treating techniques popular among other ceramic materials. Due to its beautiful remains as primary interest of many equipment designers. golden color, it has been widely used for decoration and Depends on composition and nature of the materials to be marketing purposes. It is also very hard-1770 kg/mm2, treated and their applications, heat treating may include Stable in air at temperature as high as 650-degC. It is austenitizing, quench hardening, annealing, tempering, relatively corrosion- and wear-resistant with relatively low normalizing, austempering, StreSS reliving, precipitation friction coefficient, making it very popular in cutting tool 35 hardening, Sintering, as well as Surface enhancement tech industry. Various high temperature PVD and CVD titanium niques which utilizes thermochemical treatment Such as nitride coated cutting/machine tools (Such as inserts, drills, carburizing, carbonitriding, nitriding, nitrocarburizing, etc. saws, punches, dies, molds, pins, knifes), fuel injector components are currently available in the commercial mar COMMON PRACTICES FOR CRITICAL APPLICATIONS kets. In fact, most of the above components are made of high 40 Speed tool Steel. The material itself is expensive relative to For applications involving extensive wear, the most com lower grade Steel materials. Taken diesel fuel injector com mon practices today are to chose high grade (relatively ponents as an example, the diesel fuel injection operation is expensive) Steel as starting material, for example, high speed carried out at very high pressure, normally at about 150,000 tool Steel which offers better mechanical properties Such as psi (pounds per Square inch) for diesel fuel engine. The 45 a good combination of hardneSS and toughness. After the injection is also carried out at very high Speed and in very components are machined to desired size, shape and Surface Short cycle time. The excessive failures are resulted due to finish, heat treatment is carried out to harden and temper the fatigue from repeated impact, extensive wear and erosion parts. In most cases, quench hardening may increase hard caused by abrasive particles. In order to prolong the life of the fuel injectors, high Speed tool Steel is commonly used, neSS of the treated part significantly, however, it makes the 50 part brittle. Tempering is therefore necessary to increase with extensive post-treatments, including heat treating toughness of the material, however, it Sacrifices the hard which increases hardness, tempering to relieve Stresses and neSS. It is difficult to balance between toughness and hard restore toughness, Surface nitriding, and finally coating with neSS because a part treated for maximum toughness is often titanium nitride. The entire post treatment costs approxi too Soft, whereas the same part treated for maximum hard mately three times as much as the combined cost for material 55 neSS becomes too brittle. Surface nitriding is therefore and fabrication process (including finish grounding). The employed to further improve the hardneSS and wear titanium nitride coating alone costs almost half of the total resistance. Due to the increasing Safety and environmental components. The key for cost-reduction is to lower post concerns, gas nitriding and plasma nitriding have been treatment cost, especially coating cost. widely used today. In the plasma nitriding process, nitrogen 60 containing gas (nitrogen, ammonia) is dissociated and ion NITRIDING, CARBURIZING, AND ized. The nitrogen ions bombard metal Surface, react and CARBONITRIDING diffuse into the Subsurface to form nitrided layer. The high There are basically two major kinds of nitriding methods: energy plasma used in plasma nitriding (or ionitriding) also gas phase nitriding and liquid bath nitriding. In the gas phase reduces Substrate temperature. nitriding proceSS, nitrogen-containing gases, mostly ammo 65 After nitriding, a thin film of titanium nitride is often nia or nitrogen are used. Under high temperature or high further applied to increase the hardness of the components. energy radiation, e.g. DC electric, RF radiation, ammonia or Since current titanium nitride coating techniques require US 6,482.476 B1 3 4 high temperature, all problems associated with this Development of low temperature PVD processes has been technique, as described in the previous Sections, become attempted, one of the major problems is that adhesion inevitable. between the coating and the Substrate is too weak for For certain applications Such as machining, ceramic mate wear-related applications rials are often employed by utilizing the hardness of ceramic materials.
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