throbber

`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Samsung Electronics Co., Ltd. v. Demaray LLC
`Samsung Electronic's Exhibit 1011
`Exhibit 1011, Page 1
`
`

`

`
`5,942,089
`Page 2
`
`
`
`
`OTHER PUBLICATIONS
`
`
`
`
`
`
`
`
`W. D. Sproul, P. J. Rudnik and M. E. Graham, The Effect of
`
`
`
`
`
`
`
`N.Partial Pressure, Deposition Rate and Substrate Bias
`
`
`
`
`
`
`
`Potential on the Hardness and Texture of Reactively Sput-
`
`
`
`
`
`
`
`tered TiN Coatings, Surface and Coatings Technology,
`
`
`
`39/40 (1989) 355-363.
`
`
`
`
`
`
`
`
`X. Chu, M.S. Wong, W. D. Sproul, S. L. Rohde and S. A.
`
`
`
`
`
`
`Barnett, Deposition and Properties of Polycrystalline TiN/
`
`
`
`
`
`
`
`NbN Superlattice Coatings, J. Vac Sci. Technol. A 10(A4),
`
`
`Jul./Aug. 1992.
`
`
`
`
`
`
`William D. Sproul, Control ofA Reactive Sputtering Process
`
`
`
`
`
`
`
`
`For Large Systems, Presented at
`the Society of Vacuum
`
`
`
`
`
`
`
`Coaters 36th Annual Technical Conference, Dallas, Texas,
`
`
`
`Apr. 30, 1993.
`
`
`
`
`
`
`
`
`J. Affinito and R. R. Parsons, Mechanisms of Voltage
`
`
`
`
`
`Controlled, Reactive, Planar Magnetron Sputtering of Al in
`
`
`
`
`
`
`
`At/N, and AR/O, Atmospheres, J. Vac. Sci. Technol. A 2(3),
`
`
`Jul-Sep. 1984.
`
`
`
`
`
`
`
`
`
`S. Schiller, K. Goedicke, J. Reschke, V. Kirchhoff, S.
`
`
`
`
`
`
`
`Schneider and F. Milde, Pulsed Magnetron Sputter Technol-
`
`
`
`
`
`
`
`ogy, Surface and Coatings Technology, 61 (1993) 331-337.
`
`
`
`
`
`
`
`
`P. Frach, U. Heisig, Chr. Gottfried and H. Walde, Aspects
`
`
`
`
`
`
`
`and Results of Long—Term Stable Deposition of Al,O, With
`
`
`
`
`
`
`
`High Rate Pulsed Reactive Magnetron Sputtering, Surface
`
`
`
`
`
`and Coatings Technology, 59 (1993) 177-182.
`
`
`
`
`
`
`W. D. Sproul, M. E. Graham, M. S. Wong, S. Lopez, and D.
`
`
`
`
`
`
`
`Li, Reactive Direct Current Magnetron Sputtering of Alu-
`
`
`
`
`
`
`
`minum Oxide Coatings. J. Vac. Sci. Technol. A 13(3),
`
`
`May/Jun. 1995.
`
`
`
`
`
`
`
`William D. Sproul, Michael E. Graham, Ming—Show and
`
`
`
`
`
`
`
`Paul J. Rudnik, Reactive DC Magnetron Sputtering of the
`
`
`
`
`
`
`
`
`Oxides of Ti, Zr, and Hf, Presented at
`the International
`
`
`
`
`
`
`
`Conference on Metallurgical Coatings and Thin Films,
`
`
`
`
`
`
`
`
`Town and Country Hotel, San Diego, California, Apr. 24-28,
`
`
`
`
`
`
`
`
`1994 and Submitted for publication in Surface and Coatings
`
`Technology.
`
`Ex. 1011, Page 2
`
`Ex. 1011, Page 2
`
`

`

`U.S. Patent
`
`Aug.24, 1999
`
`Sheet 1 of 5
`
`5,942,089
`
`CV
`
`vé
`
`ve
`
`A2{JOL}UODBU}JO
`}ULOd19SdU}OL
`
`12}QWOLAdS
`
`SSeOW
`
`
`
`ZE—|19M0dPas|Nnd’d'd
`
`
`
`JUNOSLUL]SUOD
`
`Ex. 1011, Page 3
`
`
`
`
`
`waishsHuiuayindsjoW;eWUaYIS
`
`rls
`
`Ex. 1011, Page 3
`
`
`

`

`U.S. Patent
`
`Aug. 24, 1999
`
`Sheet 2 of 5
`
`5,942,089
`
`oO
`
`OW
`
`N
`
`g
`
`o) ©
`“Ny
`a
`mi
`“n
`E
`Oo
`oF
`
`_O
`2
`
`O08 0000000 0 0
`Oo OO oO
`O00 0 0
`
`O
`
`Aabe LOA aBpoyyed
`
`Ex. 1011, Page 4
`
`wo
`
`3
`
`Qu
`
`O)
`O°
`oO
`)
`2
`mp)
`C
`-_

`
`O2 m
`
`M
`oO
`LY
`=
`QJ

`OH
`~ &
`E
`
`Mm
`
`Ex. 1011, Page 4
`
`

`

`U.S. Patent
`
`Aug.24, 1999
`
`Sheet 3 of 5
`
`5,942,089
`
`
`
`
`
`LOMOOGPasingavjodigdulaWWwASY
`
`‘aut|08OL09OSOrOFO2~ObO
`
`oasn
`
`TTTO
`
`OOL
`
`OOl-
`
`OOC-
`
`OOE-
`
`OOS-
`
`OOb-°
`
`A\‘abeljoA apoyyed
`
`Fold
`
`
`
`SqpasingsejodigdujauwAsy,“S1a}jaSP+a4n0g
`
`
`
`
`
`
`
`AN‘220}S2Y90Y“|INZ'21ONYOO)INF
`
`
`
`
`
`Ex. 1011, Page 5
`
`Ex. 1011, Page 5
`
`

`

`U.S. Patent
`
`
`
`
`
`
`
`SINSS21g|eleguabAxo'snabeyon196s0)-*“OIyv
`
`"+00
`
`VOls
`
`o0gaGHuise2i0eq-7-©Gursedidu|<2OSE®.<
`go1090GOvo¢€020#10Oo
`
`OS2
`
`—>
`
`Aug.24, 1999
`
`Sheet 4 of 5
`
`5,942,089
`
`
`
`MOLW2LNssatdfeltedUaBAxO
`
`Ex. 1011, Page 6
`
`Ex. 1011, Page 6
`
`

`

`U.S. Patent
`
`Aug. 24, 1999
`
`Sheet 5 of 5
`
`5,942,089
`
`4
`
`oI
`
`To)
`wv
`
`Oo
`C
`
`5
`
`OF
`=
`3
`Lie
`c
`oS
`"S&S
`
`0
`
`|
`|
`
`eg
`Oo
`
`Ex. 1011, Page 7
`
`™
`Mme
`f
`Ss
`2 ©
`£A
`on 4
`
`=O
`
`.
`
`:
`
`\
`s
`
`og
`a
`
`_
`aN
`
`S
`
`K
`
`=
`Oo
`Le
`
`©¥
`
`_)
`w~
`Q)
`.
`Oo.
`x

`OC
`oO
`c
`te)
`WO
`.
`O ™
`— y
`UL x

`x
`
`I
`
`O<
`
`oO

`
`nN
`oO
`
`—
`oO
`
`LIQ] SINSSAig JeLUe4 USDAXO
`
`Ex. 1011, Page 7
`
`

`

`
`1
`METHOD FOR SPUTTERING COMPOUNDS
`
`
`
`ON A SUBSTRATE
`
`
`BACKGROUND OF THE INVENTION
`
`
`
`
`2
`
`
`
`
`
`
`
`
`Sputtering techniques for the application of pure metals
`
`
`
`
`
`
`
`
`are fairly well refined and effective. Additionally, sputtering
`
`
`
`
`
`
`techniques for conductive or non-insulating compounds
`
`
`
`
`
`
`
`have been somewhat successful utilizing the techniques
`
`
`
`
`
`
`described in the aforesaid publications. However, certain
`
`
`
`
`
`
`
`
`Briefly,
`the present invention relates to a method and
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`materials, which provide an insulating, hard coating upon a
`apparatus for sputtering of a thin film of a compound onto
`
`
`
`
`
`
`
`
`
`
`
`substrate are difficult
`to apply as a film or may not be
`
`
`
`
`
`
`
`a substrate workpiece by means of cathodic, magnetron
`
`
`
`
`
`
`
`
`efficiently applied using such sputtering techniques. Alumi-
`sputtering.
`
`
`
`
`
`
`
`
`
`num oxide, for example, has heretofore been applied by
`
`
`
`
`
`
`Application of metals and metallic compounds by use of
`
`
`
`
`
`
`sputtering techniques to a substrate at only a small fraction
`
`
`
`
`
`
`
`
`
`a reactive deposition process is knownandisthe subject, for
`
`
`
`
`
`
`
`
`of the rate and efficiency of the application associated with
`
`
`
`
`
`
`
`
`example, of U.S. Pat. No. 4,428,811, “Rapid Rate Reactive
`
`
`
`
`
`
`
`
`
`the pure aluminum metal. Thus, low deposition rates of
`
`
`
`
`
`
`
`
`Sputtering Of A Group IVB Metal” issued Jan. 31, 1984,
`
`
`
`
`
`
`
`insulating or non-conductive metal compounds have con-
`
`
`
`
`
`
`
`incorporated herewith by reference. U.S. Pat. No. 4,428,811
`
`
`
`
`
`
`
`tinued to pose a challenge. Publications that reflect research
`
`
`
`
`
`
`
`
`discloses a method and apparatus for rapid rate deposition of
`
`
`
`
`
`
`
`
`regarding the sputtering of such compounds include the
`
`
`
`
`
`
`
`metallic compoundssuchas titanium nitride onto a substrate
`
`
`
`
`
`
`following, which are incorporated herewith by reference:
`
`
`
`
`
`
`
`
`in a vacuum chamber. In the process, the chamberis filled
`
`
`
`
`
`
`
`9. “Aspects and Results of Long-Term Stable Deposition
`
`
`
`
`
`
`
`
`
`
`with inert gas that is ionized and bombards the metal target
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`of AlL,O, with High Rate Pulsed Reactive Magnetron
`within the chamber to initiate the sputtering process. A
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Sputtering,” published in Surface and Coatings Technology,
`substrate is positioned within the chamber for coating, and
`20
`1993;
`
`
`
`
`
`
`
`
`
`
`a second reactive gas is fed into the chamber at a measured
`rate to combine at the substrate with the atomized metal
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`10. “Reactive Direct Current Magnetron Sputtering of
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`from the target to form the coating. Control systems for such
`Aluminum Oxide Coatings,” J. Vac. Sci. Technol. A 13(3),
`
`
`
`
`
`
`
`
`
`
`
`sputtering operations are also disclosed in the aforesaid
`May/June 1995; and
`
`patent.
`
`
`
`
`
`
`11. “Reactive DC Magnetron Sputtering of the Oxides of
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Overthe years, the technology associated with sputtering
`Ti, Zr, and Hf,” presented at the International Conference on
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`processes has been improved so that additional compounds
`Metallurgical Coatings and Thin Films, Town and Country
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`and materials can be applied to a substrate by. A series of
`Hotel, San Diego, Calif., Apr. 24-28, 1995, and accepted for
`
`
`
`
`
`
`
`
`
`
`
`
`papers by the co-inventorreflect research in this area includ-
`publication in Surface and Coatings Technology.
`
`
`
`ing the following:
`
`
`
`
`
`
`
`In sum,there has remained a need to provide an improved
`
`
`
`
`
`
`
`
`
`
`
`
`
`1. “High Rate Reactive Sputtering Process Control,”
`method and apparatus for the deposition of metallic, insu-
`
`
`
`
`
`
`
`
`
`
`
`published in Surface and Coatings Technology, 1987;
`lating compounds such as aluminum oxide, on a substrate
`
`
`
`
`
`
`
`
`
`
`
`
`using sputtering techniques.
`2. “The Effect of Target Power on the Nitrogen Partial
`
`
`
`
`
`
`
`Pressure Level and Hardness of Reactively Sputtered Tita-
`SUMMARYOF THE INVENTION
`
`
`
`
`
`
`
`
`
`
`nium Nitride Coatings,” published in Thin Solid Films,
`
`
`
`
`
`
`
`1989;
`
`In a principal aspect, the present invention comprises a
`
`
`
`
`
`
`
`
`
`
`
`
`method for deposition of various compounds, especially
`3. “Advancesin Partial-Pressure Control Applied to Reac-
`
`
`
`
`
`
`
`
`
`
`
`
`insulating, metallic compounds such as aluminum oxide, on
`tive Sputtering,” published in Surface and Coatings
`
`
`
`
`
`
`
`
`
`a substrate as a thin film by sputtering techniques utilizing
`Technology, 1989;
`
`
`
`
`
`
`
`
`a pulsed, constant power, direct current electric power
`
`
`
`
`
`
`
`
`4. “The Effect of N., Partial Pressure, Deposition Rate and
`Substrate Bias Potential on the Hardness and Texture of
`
`
`
`
`
`
`
`supply to cause ionization of an inert gas that bombards a
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`target thereby releasing the atomsofthe target into a vacuum
`Reactively Sputtered TIN Coatings,” published in Surface
`
`
`
`
`
`
`
`
`
`
`
`
`
`chamber and further controlling the rate of admission and
`and Coatings Technology, 1989;
`
`
`
`
`
`
`
`
`
`thus the reaction of a second, reactive gas to the chamber
`
`
`
`
`
`
`5. “Deposition and Properties of Polycrystalline TiN/NbN
`45
`
`
`
`
`
`
`
`with a combination of control signals. Specifically, the rate
`
`
`
`
`
`
`
`Superlattice Coatings,” published in J. Vac. Sci. Technol. A
`
`
`
`
`
`
`
`
`of admissionis controlled byafirst signal derived from the
`
`
`
`
`10/4, July/August 1992; and
`
`
`
`
`
`
`
`measured voltage of the target which is maintained at a
`
`
`
`
`
`
`
`
`6. “Control of a Reactive Sputtering Process for Large
`
`
`
`
`
`
`
`
`constant power setting. The rate of admission is further
`
`
`
`
`
`
`
`
`Systems,” a paper presented at
`the Society of Vacuum
`
`
`
`
`
`
`
`controlled by a second signal derived from the measured
`
`
`
`
`
`
`
`Coaters, 36th Annual Technical Conference, Dallas, Tex.,
`
`
`
`
`
`
`
`
`
`partial pressure of the reactive gas. The partial pressure of
`
`
`
`Apr. 30, 1993.
`
`
`
`
`
`
`
`
`the reactive gas is sensed by means such as an optical gas
`
`
`
`
`
`
`The text of these publications is incorporated herewith by
`
`
`
`
`
`
`
`controller or mass spectrometer, as well as the target voltage,
`reference.
`
`
`
`
`
`
`
`
`
`is sensed to provide control signals representative of the
`
`
`
`
`
`
`
`
`The energy source whicheffects the ionization of the inert
`
`
`
`
`
`
`
`desired composition and physical characteristics of the thin
`
`
`
`
`
`
`
`
`
`gas in a sputtering system has evolved overtime so that now
`
`
`
`
`
`
`
`film. The desired composition and physical characteristics
`
`
`
`
`
`
`
`pulsed, direct current electrical power is known to be a
`
`
`
`
`
`
`
`
`are derived empirically for given target materials, reactive
`
`
`
`
`
`
`
`preferred energy source to the target material. Publications
`
`
`
`
`
`
`
`
`
`gases and powersettings. To further enhance the thin film
`
`
`
`
`
`
`
`
`relating to this technique and technology include the fol-
`
`
`
`
`
`
`
`
`deposition process, the reactive gas at or near the substrate
`
`
`
`
`
`
`
`
`
`lowing:
`is subjected to local energy input, for example, by applying
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`7. “Mechanisms of Voltage Controlled, Reactive, Planar
`pulsed direct current to the substrate. By the method, it is
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Magnetron Sputtering of Al
`in Ar/N, and Ar/O,
`possible to carefully control the amountof reactive gas in the
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Atmospheres,” published in J. Vac. Sci. Technol. A 2(3),
`system and thereby increase the rate of deposition of the
`
`
`
`
`
`
`
`
`
`
`
`July-September 1984; and
`compound multiple times the rate of deposition using prior
`
`
`
`
`
`
`
`
`8. “Pulsed Magnetron Sputter Technology,” published in
`sputtering techniques.
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Surface and Coatings Technology, 1993.
`it
`is an object of the invention to provide an
`Thus,
`
`
`
`
`
`
`
`
`
`
`
`
`These publications are incorporated herewith by refer-
`improved method and apparatus for deposition of com-
`ence.
`
`
`
`
`pounds on a substrate by sputtering techniques.
`
`
`5,942,089
`
`
`
`
`
`
`
`10
`
`15
`
`
`
`25
`
`
`
`30
`
`
`
`35
`
`
`
`40
`
`
`
`
`
`
`50
`
`
`
`55
`
`
`
`60
`
`
`
`65
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Ex. 1011, Page 8
`
`Ex. 1011, Page 8
`
`

`

`
`3
`
`
`
`
`
`
`
`
`
`
`It
`is a further object of the invention to provide an
`
`
`
`
`
`
`
`
`improved method for deposition by sputtering of com-
`
`
`
`
`
`
`pounds including oxides, nitrides,
`fluorides, sulfides,
`
`
`
`
`
`chlorides, borides and mixtures thereof.
`
`
`
`
`
`
`Another object of the invention is to provide an improved
`
`
`
`
`
`
`
`
`and highly efficient method and apparatus for deposition of
`
`
`
`
`
`
`insulating, metal compounds on a substrate utilizing
`
`
`
`improved control techniques.
`
`
`
`
`
`
`Another object of the invention is to provide an improved
`
`
`
`
`
`
`
`
`
`method for deposition of thin films of insulating, metal
`
`
`
`
`
`
`compounds on a substrate at rates which are multiples of the
`
`
`
`
`
`rates of prior art sputtering techniques.
`
`
`
`
`
`
`Another object of the invention is to provide an improved
`
`
`
`
`
`
`
`
`method for deposition of metal and semi-conductor com-
`15
`
`
`
`
`
`
`poundsas thin films using sputtering techniques.
`
`
`
`
`
`
`A further object of the invention is to provide a method for
`
`
`
`
`
`
`effecting efficient deposition of compounds by sputtering
`
`
`
`
`
`
`
`techniques utilizing a constant power, pulsed direct current
`
`
`
`
`
`
`
`
`
`
`powersupply for the target material and control signals for
`
`
`
`
`
`
`
`
`controlling the admission of reactive gas wherein one signal
`
`
`
`
`
`
`
`
`
`
`
`is reflective of the voltage of the target power source and
`
`
`
`
`
`
`
`
`
`another signal is reflective of the partial pressure of the
`
`
`
`
`
`
`
`
`reactive gas used in the practice of the process.
`
`
`
`
`
`
`
`
`
`These and other objects, advantages and features of the
`
`
`
`
`
`
`
`
`
`
`invention will be set forth in the detailed description as
`follows.
`
`BRIEF DESCRIPTION OF THE DRAWING
`
`
`
`
`
`
`
`
`
`
`
`
`In the detailed description which follows, reference will
`
`
`
`
`
`
`
`
`be made to the drawing comprised of the following figures:
`FIG. 1 is a schematic of a vacuum chamber and the
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`control circuitry associated therewith for the practice of the
`
`
`
`method of the invention;
`
`
`
`
`
`FIG. 2 is a graph depicting a symmetric, bipolar pulsed,
`
`
`
`
`
`direct current power supply wave;
`
`
`
`
`
`FIG. 3 is a graph depicting an asymmetric, bipolar pulsed
`
`
`
`
`
`direct current power supply wave;
`
`
`
`
`
`FIG. 4 is a graph depicting the target voltage/oxygen
`
`
`
`
`
`
`
`partial pressure hysteresis curve for the reactive sputtering
`
`
`
`
`
`
`of aluminum in an argon/oxygen atmosphere; and
`
`
`
`
`
`
`FIG. 5 is a graph depicting the oxygen reactive gas
`
`
`
`
`
`
`
`flow/oxygenpartial pressure hysteresis curve for the reactive
`
`
`
`
`
`sputtering of aluminum in an argon/oxygen atmosphere;
`DESCRIPTION OF THE PREFERRED
`
`
`EMBODIMENT
`
`
`
`
`
`Overview And General Description
`The method of the invention as well as the associated
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`apparatus are designed to optimize the conditions for reac-
`
`
`
`
`
`
`
`
`tion between atomized target material and reactive gas to
`
`
`
`
`
`
`
`form and deposit a thin film compound in a sputtering
`
`
`
`
`
`
`
`
`
`system. Thus referring to FIG. 1 ,
`there is depicted the
`
`
`
`
`
`
`
`componentparts of a sputtering system used to practice the
`invention.
`
`
`
`
`
`
`
`Avacuum chamber10 is evacuated by a pump 12 after a
`
`
`
`
`
`
`
`
`
`
`substrate material 14, e.g. quartz or a piece of steel
`is
`
`
`
`
`
`
`
`
`mounted on a holder 16 within the chamber 10. A target
`
`
`
`
`
`
`
`
`material 18, e.g. Aluminum or some other metal or semi-
`
`
`
`
`
`
`
`
`conductor material, is also mounted within the chamber10.
`
`
`
`
`
`
`
`
`
`The target 18 serves as a cathode in the process and the
`inside walls 20 of chamber 10 serve as an anode. An inert
`
`
`
`
`
`
`
`
`
`
`
`
`
`gas, e.g. Argon (An),
`is admitted to chamber 10 from a
`
`
`
`
`
`
`
`
`
`source 22 via a meter 24 and valve 26 controlled by a
`
`
`
`
`
`controller 28 responsive to a pressure sensor 30.
`
`
`
`
`
`
`
`The target 18 is subject to a bipolar, pulsed, direct current
`
`
`
`
`
`
`
`
`
`power source 32 of the type generally knownin the art. The
`
`10
`
`20
`
`25
`
`30
`
`35
`
`
`
`
`
`
`
`
`
`
`
`40
`
`45
`
`50
`
`55
`
`60
`
`65
`
`
`
`5,942,089
`
`
`
`
`4
`
`
`
`
`
`source 32 is preferably asymmetric as depicted in FIG. 3
`
`
`
`
`
`
`
`with the cathode negatively biased, although a symmetric
`
`
`
`
`
`
`source 32, as depicted in FIG. 2, may be utilized.
`
`
`
`
`
`
`
`
`A reactive gas, such as oxygen,is provided from a source
`
`
`
`
`
`
`
`
`
`34 through a flow meter 36 and control valve 38 via a
`
`
`
`
`
`
`
`conduit 40 to the vicinity of the target 18 whereits proximity
`
`
`
`
`
`
`
`
`
`to atoms from the target will enhance reaction therewith. The
`
`
`
`
`
`
`
`reactive gas control valve 38 is responsive to a plurality of
`
`
`
`
`
`
`
`sensing or feedback signals which are input to a controller
`
`
`
`
`
`
`
`
`42 which, upon proper processing, provides a control signal
`via link 44 to valve 38.
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`The signals to the controller 42 are derived from two
`
`
`
`
`
`
`
`
`
`sources, first
`the voltage of the target 18 is constantly
`
`
`
`
`
`
`
`
`monitored. Second,the partial pressure of the reactive gas is
`
`
`
`
`
`
`
`
`monitored. Regarding the voltage target 18, this voltage may
`
`
`
`
`
`
`
`
`vary since the power to the target 18 is maintained at a
`constant value. For each set of conditions within the
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`chamber, therefore, for a given target and reactive gas,it is
`
`
`
`
`
`
`
`
`possible to derive the relationship between such constant
`
`
`
`
`
`
`
`
`
`
`power voltage and the partial pressure of the reactive gas
`
`
`
`
`
`
`
`
`thereby identifying the optimal range of partial pressure and
`
`
`
`
`
`
`
`
`voltage for formation of the compound comprised of the
`
`
`
`
`
`
`
`
`target material and reactive gas. An example of this empiri-
`
`
`
`
`
`
`cal derivation is depicted in FIG. 4 for a target material of
`
`
`
`
`
`
`aluminum in an argon/oxygen atmospherefor increasing and
`
`
`
`
`
`
`
`
`decreasing oxygen partial pressure wherein the target power
`
`
`
`
`
`
`
`
`was 2 kilowatts from a 20 kHz, pulsed direct current source
`
`
`
`
`
`
`
`
`
`
`and the total chamberpressure was 4 mTorr. Note that partial
`
`
`
`
`
`
`
`
`pressure of about 0.03 mTorrat a target voltage of 270 to 380
`
`
`
`
`
`
`
`
`volts is indicative of highly efficient film formation. This
`
`
`
`
`
`
`information or information of this type is derived from an
`
`
`
`
`
`
`
`
`experimental ortest run, and the results are programmed into
`
`
`
`
`
`
`controller 42 thus enabling the controller 42 the capability to
`
`
`
`
`
`
`provide almost
`instantaneous feedback control
`input
`
`
`
`
`
`
`because voltage measurements provided to the controller 42
`
`
`
`
`
`
`
`
`
`from target 18 are inherently rapid. Thus, the voltage feed-
`
`
`
`
`
`
`
`back signal provides a highly sensitive, rapid response,
`
`
`
`
`
`
`
`
`
`control function, when empirical or full range test run,
`
`
`
`
`
`
`
`hystersis information derived from an experiment or full
`
`
`
`
`
`
`
`
`range test run of the type reflected by FIG. 4 is programmed
`into the controller 42.
`
`
`
`
`
`
`
`
`
`
`
`
`Simultaneous with the rapid control signal derived from
`
`
`
`
`
`
`
`
`
`the voltage of target 18, a second less rapid signal is derived
`
`
`
`
`
`
`
`by directly measuring the partial pressure of the reactive gas,
`
`
`
`
`
`
`
`e.g. oxygen. Thus, as depicted in FIG. 1, a mass spectrom-
`
`
`
`
`
`
`
`
`eter 46, for example, or a partial pressure controller, e.g. an
`
`
`
`
`
`
`
`analyzer (OGC made by Leybold Infilon of East Syracuse,
`
`
`
`
`
`
`
`
`N.Y.) is provided to determine the partial pressure of the
`
`
`
`
`
`
`
`
`
`specific reactive gas. Note the signal derived from sensor 46
`
`
`
`
`
`
`
`
`
`is species specific, e.g. oxygen; whereas the target voltage
`
`
`
`
`
`
`
`
`signal is not. Thus,
`the target voltage signal, previously
`
`
`
`
`
`
`
`
`
`described, may result, at least in part, due to phenomena
`
`
`
`
`
`
`
`
`
`
`other than the partial, pressure of the reactive gas. For
`
`
`
`
`
`
`
`
`
`example, out gassing from the substrate or chamber walls
`
`
`
`
`
`
`
`
`
`may have an impact on the signal. Thus, the reactive gas
`
`
`
`
`
`
`sensor 46 provides a signal 48 to the controller which is
`
`
`
`
`
`
`
`
`
`
`reflective of the true partial pressure of the reactive gas
`
`
`
`
`
`
`
`(oxygen) albeit a slowly developed or slowly derived signal
`
`
`
`
`
`
`
`
`
`
`relative to the target voltage signal because of the instru-
`mentation involved.
`
`
`
`
`
`
`
`
`
`
`
`
`In any event,
`the meaning of the signal 48 is also
`
`
`
`
`
`
`
`dependent upon the empirical relationship between reactive
`
`
`
`
`
`
`
`
`
`gas partial pressure and flow rate. This relationship is
`
`
`
`
`
`
`
`derived simultaneously with the empirical power voltage/
`
`
`
`
`
`
`
`partial pressure relationship discussed with regard to FIG. 4
`
`
`
`
`
`
`
`
`for each specific set of conditions. FIG. 5 is a graph
`
`
`
`
`
`
`
`
`
`depicting the relationship for the same conditions (in fact,
`
`
`
`
`
`
`
`
`derived during the same empirical experimental run) as FIG.
`4.
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`Ex. 1011, Page 9
`
`Ex. 1011, Page 9
`
`

`

`5,942,089
`
`
`5
`
`
`
`
`
`
`
`
`Referring to FIG. 5, for the reported conditions and
`
`
`
`
`
`
`
`
`
`materials, which is the same as specified for the data of FIG.
`
`
`
`
`
`
`
`
`
`4, the optimal partial pressure is in the range of about 0.02
`
`
`
`
`
`
`
`
`mTorr, at which point the oxygen flow is in the range of 15
`
`
`
`
`
`
`
`
`
`
`
`to 20 Sccm. Thus,
`the signal 48 from sensor 46 can be
`
`
`
`
`
`
`
`
`utilized to “zero” or set the controller 42 so that the target
`
`
`
`
`
`
`voltage signal to controller 42 is working from an appro-
`
`
`
`priate base line.
`
`
`
`
`
`
`
`
`One further input to the system is provided to enhance the
`
`
`
`
`
`
`
`
`film deposition process. An energy source 50 provides a
`
`
`
`
`
`
`
`
`meansfor activating the reactive gas, e.g. Oxygen,at or near
`
`
`
`
`
`
`
`
`
`the substrate 14. For example, a pulsed direct current power
`
`
`
`
`
`
`
`
`supply may be applied to the substrate 14. Other energy
`
`
`
`
`
`
`
`sources include a radio frequency voltage source, lasers,
`
`
`
`
`
`
`
`electron beams, a microwave source, or an inductively
`
`
`
`
`
`
`
`coupled plasma source. A radio frequency source of 13.56
`
`
`
`
`
`
`
`MHZ or a harmonic multiple thereof may be used. The
`
`
`
`
`
`
`
`
`energy input at the substrate 14 has the effect of enhancing
`
`
`
`
`
`
`
`
`
`the process efficiency as reflected by the data derived in
`
`
`
`
`
`
`
`FIGS. 4 and 5, by way of example, so as to increase flow rate
`
`
`
`
`and voltage at optimal conditions.
`
`
`
`
`
`
`
`
`Also by correlating the data of the type derived in FIGS.
`
`
`
`
`
`
`
`
`
`4 and 5 with various physical parameters of the film
`
`
`
`
`
`
`
`compound, it becomes possible to apply films having cus-
`
`
`
`
`
`
`
`tomized characteristics. For example, each of the data points
`
`
`
`
`
`
`
`of FIGS. 4 and 5 are representative of compounds having
`
`
`
`
`
`
`
`associated therewith a variety of measurable physical char-
`
`
`
`
`
`acteristics including conductivity, modulus, hardness,
`
`
`
`
`
`
`extinction coefficient, index of refraction,reflectivity, trans-
`
`
`
`
`
`
`
`mission and constituent composition. By controlling the
`
`
`
`
`
`
`
`sputtering process to such data points, as it is possible to do
`
`
`
`
`
`
`
`
`
`with this process, the desired custom film may be sputter
`
`
`
`applied to a substrate 14.
`
`
`
`
`
`
`
`
`in the deposition of
`The process is especially useful
`
`
`
`
`
`
`
`insulating, metal compounds such as aluminum oxide.
`
`
`
`
`
`Experimental results demonstrate application rates 15 to 20
`
`
`
`
`
`
`
`
`
`times better than prior techniques. For example, with the
`
`
`
`
`
`reactive sputtering of stoichiometric Al,O,, the deposition
`
`
`
`
`
`
`
`
`
`rate had been increased from about 5% of the metal depo-
`
`
`
`
`
`
`
`
`sition rate to 70% or more of the metal deposition rate. Also,
`
`
`
`
`
`
`
`the process is useful with many compounds including
`
`
`
`
`
`
`oxides, nitrides, carbides, sulfides,
`fluorides, chlorides,
`
`
`
`
`
`
`
`borides and mixtures thereof. Numerous metals, including
`
`
`
`
`
`
`aluminum,titanium, hafnium, zirconium, tantalum,silicon,
`
`
`
`
`
`
`
`
`and chromium have been successfully used as the target
`material.
`
`
`
`Specific Example:
`
`
`
`
`
`
`Following is a specific example of the practice of the
`invention:
`
`
`
`
`10
`
`
`
`15
`
`
`
`20
`
`25
`
`
`
`30
`
`35
`
`
`
`40
`
`
`
`45
`
`
`
`
`
`
`
`Deposition of Aluminum Oxide by Means of
`
`
`Reactive DC Sputtering
`
`
`
`
`
`
`Aluminum oxide (stoichiometric composition but non-
`
`
`
`
`
`
`
`crystalline) may be deposited using the following deposition
`
`
`system hardware:
`
`
`
`
`
`
`
`
`The substrate to be coated is placed in a stainless steel
`
`
`
`
`
`
`
`
`vacuum chamber, approximately 29" o0.d. and about 30"
`
`
`
`
`
`
`
`high, whichis electrically groundedto earth potential and is
`
`
`
`
`
`
`
`
`
`pumped with a 6" diffusion pump and a 1500 1/s turbo-
`60
`
`
`
`
`
`
`
`
`molecular pump, which are both backed up with appropri-
`
`
`
`
`
`
`
`
`ately sized mechanical pumps(in this case, Edwards EM2-
`
`
`
`
`
`
`
`80’s) capable of achieving a base pressure of 1x10~° Torr.
`
`
`
`
`
`
`
`
`The substrate may bea flat glass slide or other material of
`
`
`
`
`
`
`
`choice, which is mounted on the 5"-diameter, rotatable
`
`
`
`
`
`
`
`
`substrate table. The closest approach of the substrate to the
`
`
`
`
`
`
`
`target is about 3" and it may berotated or held stationary
`
`
`during coating.
`
`50
`
`55
`
`65
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`6
`
`
`
`
`
`
`Two nominally 5"x15" rectangular MRCInsettargets are
`
`
`
`
`
`
`
`mounted vertically, opposing one another about 11" apart
`with the substrate table in between. The cathodes are an
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`unbalanced magnetron design, which enhances the plasma
`
`
`
`
`
`
`
`density in the vicinity of the substrate, and at least one target
`
`
`
`
`
`
`
`is aluminum with a metallic purity of at least 99.99%.
`
`
`
`
`
`
`The cathodes (targets) are each connected to Advanced
`
`
`
`
`
`Energy MDX 10 kW de power supplies through 20 kHz
`
`
`
`
`
`
`
`Sparc-Le (or higher frequency) units which together provide
`
`
`
`
`
`
`
`a pulsed de power and suppression of arcing on the target
`
`
`
`surface during sputtering.
`
`
`
`
`
`
`
`The substrate table is connected to a 3 kW rf power
`
`
`
`
`
`
`
`
`
`supply, and the induced de voltage is read out through a
`
`
`
`
`
`
`
`meter which is shielded from rf power by means of an
`
`
`appropriatefilter.
`
`
`
`
`
`
`
`The total gas pressure in the chamber is monitored by a
`
`
`
`
`
`
`Baratron (capacitance manometer) for sputtering pressures
`
`
`
`
`
`
`
`
`(1-10 mTorr), and lower pressures are monitored with a
`
`
`
`
`
`
`
`Bayard-Alpert type ionization gauge. The ionization gauge
`
`
`
`
`
`
`
`
`is also used as a reference in checking the calibration of the
`
`
`
`
`
`
`
`
`partial pressure sensors (OGC or mass spec.), or a more
`
`
`
`
`
`
`
`
`stable instrument such as a spinning rotor gauge can be used
`
`
`
`and is preferred if available.
`
`
`
`
`
`
`
`
`
`
`The partial pressures of all gases in the system are
`
`
`
`
`
`
`
`monitored with an Inficon Quadrex 100, quadrupole mass
`
`
`
`
`
`
`
`
`
`spectrometer, and two of the gases (oxygen and argon) are
`
`
`
`
`
`
`
`monitored with an Inficon OGC (Optical Gas Controller).
`
`
`
`
`
`
`The mass spectrometer is attached to a sampling system
`
`
`
`
`
`
`whichis differentially pumped,since it requires an operating
`
`
`
`
`
`
`
`
`
`
`pressure that is typically in the 10-° Torr range, and is
`
`
`
`
`
`
`
`
`
`mounted to the top of the chamber. The OGC is attached
`
`
`
`
`
`
`
`directly to the back of the chamber through a standard KF
`
`
`
`
`
`flange, since it operates at sputtering pressures.
`
`
`
`
`
`
`
`
`
`
`The gas flow controllers are MKS model 260 with modi-
`
`
`
`
`
`
`
`fications that allow them to respond to pressure signals
`
`
`
`
`
`
`
`
`
`
`instead of flow signals. In this case, the total pressure is
`
`
`
`
`
`
`
`maintained constant by a feedback control involving the
`
`
`
`
`
`
`
`
`
`Baratron and the MKScontroller. The target voltage on the
`
`
`
`
`
`
`
`aluminum target is used as the primary indicator of oxygen
`
`
`
`
`
`
`
`partial pressure during sputtering and is used as a feedback
`
`
`
`
`
`
`
`
`
`signal to the MKScontroller which operates the inlet valve
`
`
`
`
`
`
`
`for a quick response to any deviations in partial pressure
`
`
`
`
`
`
`
`
`(voltage). Since the voltage is not a unique signal with
`
`
`
`
`
`
`
`
`
`respect to the partial pressure of oxygen, the OGC or the
`
`
`
`
`
`
`
`mass spectrometer is used to provide a feedback signal for
`
`
`
`
`
`
`
`
`
`
`the voltage set point, which is thus tied to the actual desired
`
`
`
`
`
`
`
`
`
`level of oxygen partial pressure. This OGC or mass spec-
`
`
`
`
`
`
`
`
`
`trometer value is updated more slowly than the voltage. This
`
`
`
`
`
`
`
`
`dual feedback loop provides a fast response that optimizes
`
`
`
`
`
`
`
`the process control and maintains a unique relationship
`
`
`
`
`
`
`
`
`
`between the control set points and the selected partial
`
`
`pressure of oxygen.
`
`
`
`
`
`
`
`
`In order for the process to function in the preferred
`
`
`
`
`
`
`
`
`manner, one desires to also establish an anode surface in
`
`
`
`
`
`
`
`close proximity to the plasma but shielded from deposition,
`
`
`
`
`
`
`
`
`since the insulating film produced in the process will cause
`
`
`
`
`
`
`the anode to become non-functional if not protected and
`
`
`
`
`
`would cause the process to stop.
`
`
`Deposition protocol:
`
`
`
`
`
`
`
`
`The appropriate partial pressure of oxygen has been
`
`
`
`
`
`
`
`
`previously selected from an initial determination of the
`
`
`
`
`
`
`
`
`
`
`hysteresis curve, which relates the gas flow (see FIG. 5) and
`
`
`
`
`
`
`
`
`
`the target voltage (see FIG. 4) to the set partial pressure of
`
`
`
`
`
`
`
`oxygen in a fixed and determinable way for a given system
`
`
`
`
`
`
`
`
`and given operating conditions. The partial pressure that is
`selected will be that which uses the least amountof reactive
`
`
`
`
`
`
`
`
`
`
`Ex. 1011, Page 10
`
`Ex. 1011, Page 10
`
`

`

`
`
`5,942,089
`
`
`7
`
`
`
`
`
`
`
`
`
`gas and still makes a coating with the desired properties.
`
`
`
`
`
`
`
`
`
`Once the partial pressure of O, has been determined that
`
`
`
`
`
`
`
`
`corresponds to the desired properties of the oxide coating
`
`
`
`
`
`
`
`
`
`
`(e.g., optically clear), and the target voltage for that partial
`
`
`
`
`
`
`
`
`
`pressure is known, the necessary set points for the process
`5
`
`
`
`
`
`can be inserted into the controllers.
`
`
`
`
`
`
`The following operating parameters areset:
`
`
`
`

This document is available on Docket Alarm but you must sign up to view it.


Or .

Accessing this document will incur an additional charge of $.

After purchase, you can access this document again without charge.

Accept $ Charge
throbber

Still Working On It

This document is taking longer than usual to download. This can happen if we need to contact the court directly to obtain the document and their servers are running slowly.

Give it another minute or two to complete, and then try the refresh button.

throbber

A few More Minutes ... Still Working

It can take up to 5 minutes for us to download a document if the court servers are running slowly.

Thank you for your continued patience.

This document could not be displayed.

We could not find this document within its docket. Please go back to the docket page and check the link. If that does not work, go back to the docket and refresh it to pull the newest information.

Your account does not support viewing this document.

You need a Paid Account to view this document. Click here to change your account type.

Your account does not support viewing this document.

Set your membership status to view this document.

With a Docket Alarm membership, you'll get a whole lot more, including:

  • Up-to-date information for this case.
  • Email alerts whenever there is an update.
  • Full text search for other cases.
  • Get email alerts whenever a new case matches your search.

Become a Member

One Moment Please

The filing “” is large (MB) and is being downloaded.

Please refresh this page in a few minutes to see if the filing has been downloaded. The filing will also be emailed to you when the download completes.

Your document is on its way!

If you do not receive the document in five minutes, contact support at support@docketalarm.com.

Sealed Document

We are unable to display this document, it may be under a court ordered seal.

If you have proper credentials to access the file, you may proceed directly to the court's system using your government issued username and password.


Access Government Site

We are redirecting you
to a mobile optimized page.





Document Unreadable or Corrupt

Refresh this Document
Go to the Docket

We are unable to display this document.

Refresh this Document
Go to the Docket