Source: https://patents.justia.com/patent/8911528
Timestamp: 2019-01-17 06:34:27
Document Index: 176935362

Matched Legal Cases: ['Application No. 10194969', 'Application No. 10', 'Application No. 10194969', 'Application No. 10194969', 'Application No. 95138492', 'Application No. 95138492', 'Application No. 10']

US Patent for Methods of making molybdenum titanium sputtering plates and targets Patent (Patent # 8,911,528 issued December 16, 2014) - Justia Patents Search
Justia Patents Consolidated Metal Powder CompositionsUS Patent for Methods of making molybdenum titanium sputtering plates and targets Patent (Patent # 8,911,528)
Nov 2, 2010 - H.C. Starck Inc.
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This application is a divisional application of U.S. application Ser. No. 11/255,018 filed on Oct. 20, 2005 which is incorporated by reference in its entirety.
Various sputtering techniques are used in order to effect the deposition of a film over the surface of a substrate. Deposited metal films, such as metal films on a flat panel display device, can be formed by a magnetron sputtering apparatus or other sputtering techniques. The magnetron sputtering apparatus induces plasma ions of a gas to bombard a target, causing surface atoms of the target material to be ejected and deposited as a film or layer on the surface, of a substrate. Conventionally, a sputtering source in the form of a planar disc or rectangle is used as the target, and ejected atoms travel along a line-of-sight trajectory to deposit on top of a wafer whose deposition face is parallel to the erosion face of the target. Tubular-shaped sputtering targets can also be used, as described in co-pending application Ser. No. 10/931,203.
In an additional aspect, the present invention provides a method of preparing a molybdenum-titanium sputtering target having a single β(Ti, Mo) phase, the method comprising the steps of:
Titanium powder (Grade Ti-050, 100/325 mesh from Micron Metals) and molybdenum powder (MMP-7, −100 mesh, from H.C. Starck) were blended in a V-blender in proportions to achieve 33.3% Ti (by weight). Blending time was adjusted to achieve uniform distribution. No protective atmosphere was used during blending or discharging of the blenders.
Samples were cut from each of the test billets and evaluated for density, microstructure by metallographic examination and SEM-EDS, and hardness. Density results are summarized, in Table 1. Densities, as measured by the Archimedes method, from Vendor B followed predicted behavior; however, densities of samples HIP'd at Vendor A were lower than expected and showed non-uniform deformation.
680° C. 690° C. 750° C. 825° C. 925° C. 950° C. 1038° C. 1040° C.
Vendor B 6.73 7.14 7.22 7.27 Vendor A 6.2 6.5 6.52 6.99 7.10
TABLE 2 Densification response at 15,000 psi for 8 hours
HIP temperature 725° C. 750° C. 780° C. Density (g/cc) 7.05 7.11 7.14
Concurrently, a large block of MoTi was CIP'd at 19,000 psi by Vendor A to 6.8″ by 6¾″ by 17¼″ and about 65% dense (4.78 g/cc) and HIP'd for four hours at 15,00 psi and 750° C. to finish at a size of approximately 5¾″ by 5½″ by 15½″ (5.697″×5.425″×15.406″ at its smallest dimensions).
Blended Mo and Ti powders at a ratio of 50 atomic percent each were cold isostatically pressed to approximately 65% to 75% theoretical density to form a block approximately 6-in. by 6-in. by 20-in. and encapsulated in a steel can using methods known in the art. The powder-filled can was hot isostatically pressed for four hours at 15,000 psi and 750° C. The consolidated compact was removed from the steel can and cut into slices approximately 5½-in. by 5½-in. by 1-in. Surfaces to be bonded were machined flat, and four pairs of slices were each encapsulated in steel cans as before with the bond material between the slices. The slices were oriented in the can to make a sandwich approximately 2-inches thick. The bonding agents examined were: blended Mo and Ti powders at a ratio of 50 atomic percent each, Ti powder (to finish at 0.15 to 0.17-in. thick), and Ti foil (0.035-in. thick). One set of slices had nothing between them. The assemblies were hot isostatically pressed for four hours at 15,000 psi and 825° C.
TABLE 3 Bond Material Mean/ksi Std. Dev./ksi
Mo + Ti powder, 50 a/o 116.0 6.03 Ti Powder 167.5 3.88 None 111.4 13.70 Ti foil 136.0 11.08 Mo—Ti Matrix 168.1 6.81 n = 5 for each condition
The deposition on the substrates was performed on the power mode (fixed power applied to, the target) under different conditions where: gas pressure and time were varied. Table 4 lists the parameters employed.
Parameters for deposition at 1000 W, with substrate at 0 V, grounded.
1 h x x X x X ~2 min x x x
Gas pressure (mTorr) Std.
1 2 3 4 5 Avg. dev.
Target Mo—Ti on 5.85 6.04 6.43 6.28 6.55 6.23 0.255 Corning 1737 (μm/h) Target Mo—Ti on Si 5.66 5.64 6.5 6.5 6.08 0.425 (μm/h)
6. Adhesion (Tape test). Adhesion of Mo—Ti coatings was measured by tape test. Mo—Ti coatings on Corning 1737 glass with thickness around 200 nm demonstrated much better adhesion than those coatings on stainless steel and soda lime glass substrates with thickness around 5 μm, possibly due to better chemical, bonding and smaller total stress.
Tape test results of Mo—Ti coatings with thickness around 200 nm on Corning 1737 glass substrates
1 mTorr 3 mTorr 5 mTorr Target Mo—Ti 5B 5B 5B
Tape test results of Mo—Ti coatings with thickness around 5 μm on stainless steel and soda lime substrates.
1 mTorr 2 mtorr 3 mTorr 4 mtorr 5 mTorr Target Mo—Ti 0B 0B 1B 0B 1B on stainless steel Target Mo—Ti 0B 0B 0B 0B OB on soda lime glass
7. Etch rate. Etch rate of Mo—Ti coatings on Si substrates were measured by immersing the coatings in Ferricyanide solution at 25° C. for 30 minutes. Etch rates of Mo—Ti: coatings were lower than those of Mo—NbZr and pure Mo coatings.
Etch rate of molybdenum coatings produced at 1000 W for 1 hour, 0 V bias (grounded) in Ferricyanide solution at 25° C.
Deposition Etch rate pressure Target Mo—Ti (mTorr) (μm/min) 1 0.063 2 0.064 3 0.098 4 0.081 5 0.078 average 0.077
Sheet resistance and resistivity values for films deposited under different deposition conditions
Pressure Power Time Thickness resistance Resistivity (mTorr) (W) (s) (nm) (Ω/) (μΩ · cm)
Target 1 1000 117 179 4.45 79.6 Mo—Ti 3 1000 109 182 4.50 81.9 5 1000 108 170 4.58 78
With the decrease of deposition pressure, Mo—Ti coatings became denser. Coatings on Corning 1737 glass substrates were denser than on Si substrates. Mo—Ti coatings on Corning 1737 glass with thickness around 200 nm demonstrated much better adhesion than those coatings on stainless steel and soda lime glass substrates with thickness around 5 μm, possibly due to better chemical bonding and smaller total stress. Etch rates of Mo—Ti coatings were much lower than those of pure Mo coatings. The resistivity of Mo—Ti coatings were higher than those of pure Mo coatings. The uniformity of Mo—Ti is comparable to previous pure Mo coatings
1. A molybdenum-titanium sputtering target consisting essentially of molybdenum and titanium, wherein the concentration of any β(Mo, Ti) alloy phase is from greater than 0% up to 15% by volume, wherein the target has a density that is at least 95% of theoretical density, and wherein the sputtering target includes the titanium at a concentration of 40-60 atomic percent, based on the total number of titanium and molybdenum atoms in the sputtering target.
2. The sputtering target of claim 1, wherein the sputtering target has a thickness of 8 inches or less.
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Patent Publication Number: 20110097236
Assignee: H.C. Starck Inc. (Newton, MA)
Inventors: Mark E. Gaydos (Nashua, NH), Prabhat Kumar (Framingham, MA), Steve Miller (Canton, MA), Norman C. Mills (Phoenix, AZ), Gary Rozak (Akron, OH), Rong-Chein Richard Wu (Taipei City)
Application Number: 12/917,668
Current U.S. Class: Consolidated Metal Powder Compositions (75/228); Chromium Or Molybdenum Containing (420/421); Consolidation Of Powder Prior To Sintering (419/38)
International Classification: B22F 1/00 (20060101); B22F 3/00 (20060101); C22C 1/00 (20060101);