`Samsung Electronic's Exhibit 1004 Vol . 2
`Ex. 1004, Page 538
`
`
`
`REPLACEMENT SHEET
`Inventors: Hongmei ZHANG etal.
`Application No. 10/954,182
`Title: BIASED PULSE DC REACTIVE
`SPUTTERING OF OXIDE FILMS
`
`22/27
`
`
`
`BEST AVAILABLE Copy
`
`Ex. 1004, Page 529
`
`Ex. 1004, Page 529
`
`
`
`REPLACEMENT SHEET
`Inventors: Hongmei ZHANG etal.
`Application No. 10/954, 182
`Title: BBAASED PULSE DC REACTIVE
`SPUTTERING OF OXIDE FILMS
`
`23/27
`
`3o
`
`®
`= 38
`
`-20dBm,Expx150mw,0dBm,Exp LO
`
`oA150mw,
`
`&3
`
`&
`YS
`==
`EEoo
`B®
`
`FIG.26
`
`
`
`Wavelength(nm)
`
`oO
`w-
`
`wL
`
`O
`WwWel
`
`io
`xs
`-
`
`Ww
`w)_
`
`oW
`
`oO
`
`©o
`
`ll
`=
`
`a 5
`
`)
`
`¢@a
`
`l
`
`w i
`
`o- N - oOo
`
`ao © -M
`
`oO w
`
`wv
`
`(gp) urep
`
`+
`
`Ex. 1004, Page 530
`
`Ex. 1004, Page 530
`
`
`
`REPLACEMENT SHEET
`Inventors: Hongmei ZHANG etal.
`Application No. 10/954,182
`Title: BASED PULSE DC REACTIVE
`SPUTTERING OF OXIDE FILMS
`
`24/27
`
`dB
`
`
`
`—o— 1310 IL
`
`—i-- Gain in C-band
`
`
`
`650
`
`700
`
`750
`
`800
`
`850
`
`Annealing Temperature (c)
`
`FIG, 27
`
`Life Time and Up-conversion vs. Annealing
`Temperature
`
`
`
`Cup(cnv*75)
`
`1.20E-17
`
`1.10E-17
`
`1.00E-17
`
`9.00E-18
`
`8.00E-18
`
`7.00E-18
`
`6.00E-18
`
`5.00E-18
`
`4.00E-18
`
`3.00E-18
`
`2.00E-18
`
`
`
`
`1.00E-18
`720
`
`
`
`
`
`
` fe
`
`
`840
`
`740
`
`760
`
`780
`
`800
`
`820
`
`Anneal Temperature
`
`FIG. 28
`
`1.9
`
`1.8
`
`1.7
`
`1.6
`
`1.5
`
`1.4
`
`1.3
`
`1.2
`
`1.1
`
`(SW)
`
`Ex. 1004, Page 531
`
`Ex. 1004, Page 531
`
`
`
`REPLACEMENT SHEET
`Inventors: Hongmei ZHANG et al.
`Application No. 10/954,182
`Title: BIASED PULSE DC REACTIVE
`SPUTTERING OF OXIDE FILMS
`
`25/27
`
`1.535
`
`1.53
`
`x<
`2 1.525
`£
`
`1.52
`
`1.515
`
`index and Thickness
`
`
`
`1200
`
`1150
`
`1000
`
`1050
`
`1000
`
`950
`
`900
`
`Wafer Number
`
`§ 2000
`es|oUmhUhUlUGa
`ptc
`
`532nm PL/um
`
`@ 532nm PL/um
`
`
`
`w
`
`500
`
`
`
`0
`
`2
`
`4
`
`6
`
`8
`
`Wafer Number
`
`FIG. 30
`
`a
`
`Ex. 1004, Page 532
`
`Ex. 1004, Page 532
`
`
`
`REPLACEMENT SHEET
`Inventors: Hongmei ZHANG etal.
`Application No. 10/954,182
`Title: BAASED PULSE DC REACTIVE
`SPUTTERING OF OXIDE FILMS
`
`26/27
`
`Life Time
`
`—~ 25
`
`Lo
`”ep
`>
`2
`
`
`9)
`
`£=
`
`1.5
`
`ee ee—
`10.5pe
`
`0
`
`1.524
`
`1.5235
`
`1.523
`
`1.5225
`
`1.522
`
`1.5215
`
`1.521
`
`1.5205
`
`1.52
`
`Index
`
`0
`
`1
`
`2
`
`3
`
`4
`
`Wafer Number
`
`4500
`
`4000
`
`3500
`3000
`
`2500
`
`2000
`
`1500
`
`4000
`
`500
`
`273-1
`
`273-2)
`
`274.1
`
`274.2
`
`275.1 275.2
`
`Wafer ID
`
`FIG, 32
`
`+
`
`Ex. 1004, Page 533
`
`Ex. 1004, Page 533
`
`
`
`REPLACEMENT SHEET
`Inventors: Hongmei ZHANG etal.
`Application No. 10/954,182
`Title: BAASED PULSE DC REACTIVE
`SPUTTERING OF OXIDE FILMS
`
`27/27
`
`@Series1
`
`R.IvsO2/N2Ratio
`
`30
`
`25
`
`20
`
`15
`
`10
`
`O2/N2Ratio
`
`FIG.33
`
`1.8
`
`1.75
`
`1.7
`
`1.65
`
`1.6
`
`1.55
`
`1.5
`
`1.45
`
`1.4
`
`+
`
`Ex. 1004, Page 534
`
`Ex. 1004, Page 534
`
`
`
`PATENT
`CustomerNo. 22,852
`Attorney Docket No. 9140.0016-01
`
`6\PE
`
`
`
`Remus!
`
`
`
`DEC 21 2005
`
`%o
`
`IN THE UNITED STATES PATENT AND TRADEMARKOFFICE
`
`Group Art Unit: 2823
`
`) ) ) )
`
`) Examiner: ESTRADA;Michelle
`a
`
`Confirmation No.: 9873
`
`) ) ) )
`
`)
`
`In re Applicationof:
`
`ZHANG,Hongmeiet al.
`
`Application No.: 10/954,182
`
`Filed: October 1, 2004
`
`For:
`
`BIASED PULSE DC REACTIVE
`SPUTTERING OF OXIDE FILMS
`
`MAIL STOP AMENDMENT
`Commissioner for Patents
`P.O. Box 1450
`Alexandria, VA 22313-1450
`
`Sir:
`
`THIRD SUPPLEMENTAL INFORMATION DISCLOSURE STATEMENT
`UNDER37 C.F.R.§1.97(c
`
`Pursuant to 37 C.F.R. §§ 1.56 and 1.97(c), Applicants bring to the attention of the
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`Examiner the documents on the attachedlisting. This Information Disclosure Statementis being
`
`filed after the events recited in Section 1.97(b) but, to the undersigned's knowledge, before the
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`mailing date ofeither a Final action, Quayle action, or a Notice of Allowance. Underthe
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`provisions of 37 C.F.R. § 1.97(c), the Commissioneris hereby authorized to chargethe fee of
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`$180.00 to Deposit Account No. 06-0916 as specified by Section 1.17(p).
`
`©
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`Copiesof the listed non-patentliterature documents are attached. Copies of the U.S.
`
`patents and patent publications are not enclosed.
`
`Applicants respectfully request that the Examiner consider the listed documents and
`
`indicate that they were considered by making appropriate notations on the attached form.
`12/28/2005 SSITHIB1 00000001 060916
`10954182
`FC1806
`180.00 DA
`
`Ex. 1004, Page 535
`
`Ex. 1004, Page 535
`
`
`
`b-
`
`This submission does not represent that a search has been madeorthat no betterart exists
`
`and does not constitute an admissionthat each orall of the listed documents are material or
`
`constitute "prior art." If the Examinerapplies any of the documents as priorart against any
`claimsin the application and Applicants determine that the cited documents do not constitute
`
`"prior art” under United States law, Applicants reservethe rightto presentto the office the
`
`relevant facts and law regarding the appropriate status of such documents.
`
`Applicants further reservethe right to take appropriate action to establish the patentability
`
`of the disclosed invention over the listed documents, should one or moreof the documents be
`
`applied against the claimsof the presentapplication.
`
`If there is any fee due in connection with the filing of this Statement, please charge the
`
`fee to our Deposit Account No. 06-0916.
`
`Respectfully submitted,
`
`FINNEGAN, HENDERSON, FARABOW,
`GARRETT & DUNNER,L.L.P.
`
`
`
`Dated: December21, 2005
`
`| Express Mail Label No.
`|
`EV 758329240 US
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`|
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`-2-
`
`Ex. 1004, Page 536
`
`Ex. 1004, Page 536
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`
`
`
`EXPRESS MAIL NO. EV 758329240 US
`
`Complete if Known
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`ApplicationNumber|1064102SCSC~S
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`(Use a5 many sheets asnecessary)
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` U.S. PATENTS AND PUBLISHEDU.S. PATENT APPLICATIONS
`
`Document Number
`.
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`Examiner
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`Cite
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`Relevant Passages or Relevant
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`TT«US5,478,456 12-26-1995|Humpalet al. Po
`
`Note: Submission of copies of U.S. Patents and published U.S. Patent Applications is not required.
`
`FOREIGN PATENT DOCUMENTS
`
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`Initials"
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`i
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`.
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`Foreign Patent Document
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`Translation‘
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`“
`
`Examiner
`Initials”
`
`Cite
`No.!
`
`Translation®
`
`NON PATENT LITERATURE DOCUMENTS
`Include nameofthe author (in CAPITAL LETTERS),title ofthe article (when appropriate),title of the item (book,
`magazine, journal, serial, symposium,catalog,etc.), date, page(s), volume-issue number(s), publisher, city and/or
`country where published.
`DOREY,R.A., “Low temperature micromoulding of functional ceramic devices,” Grant
`summary for GR/S84156/01 for the UK Engineering and Physical Sciences Research Council,
`2 pages (2004).
`HOWSON,RLP., “The reactive sputtering of oxides and nitrides,” Pure & Appl. Chem.
`66(6):1311-1318 (1994).
`Office Action issued September 21, 2005 in U.S. Application No. 11/100,856 (Attorney
`Docket No. 09140.0015-01).
`Office Action issued on August 4, 2005, in U.S. Application No. 10/101,863 (Attorney Docket
`No. 09140.0016-00).
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`No. 09140-0025-00).
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`|
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`Examiner
`Signature
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`Considered
`
`EXAMINER: Initial if reference considered, whether ornotcitation is in conformance with MPEP 609. Drawline through
`citation if not in conformance and not considered.
`Include copy of this form with next communication to applicant.
`
`Ex. 1004, Page 537
`
`Ex. 1004, Page 537
`
`
`
`PATENT
`Customer No. 22,852
`Attorney Docket No. 9140.0016-01
`
`IN THE UNITED STATES PATENT AND TRADEMARKOFFICE
`
`In re Applicationof:
`
`ZHANG, Hongmeietal.
`
`Application No.: 10/954,182
`
`Filed: October 1, 2004
`
`For:
`
`BIASED PULSE DC REACTIVE
`SPUTTERING OF OXIDE FILMS
`
`MAIL STOP AMENDMENT
`Commissioner for Patents
`P.O. Box 1450
`Alexandria, VA 22313-1450
`
`Sir:
`
`SUBMISSION OF REPLACEMENT DRAWINGS
`
`Subject to the approval of the Examiner, please replace the drawingsin the
`
`above-identified application with the twenty-seven (27) sheets of drawingsfiled herewith
`
`(Figures 1A-1B, 2-15, 16A-16D, and 17-33). If the replacement drawings for any reason are not
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`If any fees are necessary for the submission of these formal drawings, please charge our
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`Deposit Account No. 06-0916.
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`Respectfully submitted,
`
`FINNEGAN, HENDERSON, FARABOW,
`
`GARRETT &, DUNNER,L.L.P.
`
`
`Gary
`J. Edwards
`Reg. No. 41,008
`
`Date: December 21, 2005
`
`By:
`
`| EXPRESS MAIL LABEL NO.
`|
`EV 758329240 US
`
`Ex. 1004, Page 538
`
`Ex. 1004, Page 538
`
`
`
` LICATION FEE DETERMINATION RECO
`
`PATENTAPP
`a
`
`Columa 1
`
`=
`
`
`
`on] *200=
`
`|
`
`
`
`
`
`(independent :
`FIRST PRESENTATION OF MULHIPLE OEPENOENT
`
`,
`
`°D afoF>2
`SO OTHER THAN
`SMALLENTITY OR SMALL ENTITY
`
`
`
`
`* (f the difference in column 1 is less than zero, enter “O" ia column 2
`‘CLAIMS ASAMENDED- PARTII
`:
`“(Columat)
`- Golumn2
`.
`HIGHEST
`" AUMBER
`REMAINING
`
`
`AFTER =|TIONALPREVIOUSLY - | .
`
`_ AMENOMENT
`PAIO.FOR
`;
`\ _
`
`
`
`
`
`RD.
`Effective December 8, 2004
`oY
`
`
`CLAIMS ASFILED-PARTI
`OTHER THAN
`SMALLENTITY
`
`
`
`TYPE [oJ OR. SMALLENTITY:
`
`
`
`
`
`
`
`
`
`
`Rate
`Basic FEE] 150.00 onfoasicFee300.00 |
`
`
`
`ronceunanGans|anes)
`
`QPa) x“4aP
`
`ncereerous|nissef|
`MULTIPLEDEPENDENT CLAIM PRESENT.
`
`
`
`“AMENDMENTA
`
`
`
`
`AMENDMENTB-
`
`
` ||Be
`
`AMENDMENTC.
`
`
`
`
`
`
`Avor
`7
`“ADOC |
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`HIGHEST.
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`REMAINING
` &UMBER
`
`| RATE | RATE|TIONALTIONAL|’
`. AFTER '
`PREVIOUSLY
`“AMENOMENT
`PALO FOR -
`,
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`
`AMENDMENT
`:
`E
`
`on
`
`Ex. 1004, Page 539
`
`Ex. 1004, Page 539
`
`
`
`Application Number
`Oo
`Apniicant(s)
`
`Fding Date
`
`isd
`
`* May be used for additional claims or amendments
`
`
` ET|ATTA
`
`CLAIMS ONLY
`
`AS FILED
`
`ceIDMENT
`
`nNs™hoomcoBS~==AIR~87.a80=Ele&
`
`Ctaims
`
`.~SpdfTo
`ztALLeee
`AOATeetUUUAASIAVINSeSrerteUGAAAAIOSE7?--0=-tpArrrecoertATT
`oemTTTTnSAUT
`rereadHEETTTTEEPEetreeeL|AATTETTTTELELLEEEeeetere
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`
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`yfAUTereTTTTTTTTTSis
`Eosersicuillsaziesecevenerex
`ALTET
`
`Ex. 1004, Page 540
`
`Ex. 1004, Page 540
`
`
`
`
`
`
`
`
`
`
`
`~
`
`PS-OP 6-2 6
`
`Lipa
`
` IN THE UNITED STATES PATENT AND TRADEMARKOFFICE
`
`PATENT
`Customer No. 22,852
`Attorney Docket No. 9140.0016-01
`
`,
`
`M
`
`Group Art Unit: 2823
`
`Examiner: ESTRADA,Michelle
`
`Confirmation No.: 9873
`
`) ) ) ) ) ) ))
`
`__)
`
`In re Application of:
`
`ZHANG,Hongmeiet al.
`
`Application No.: 10/954,182
`
`Filed: October 1, 2004
`
`For:
`
`BIASED PULSE DC REACTIVE
`SPUTTERING OF OXIDEFILMS
`
`~
`
`MAIL STOP AMENDMENT
`Commissioner for Patents
`P.O. Box 1450
`Alexandria, VA 22313-1450
`
`Sir:
`
`FOURTH SUPPLEMENTAL INFORMATION DISCLOSURE STATEMENT
`UNDER 37 C.F.R.§ 1.97(c)
`
`Pursuant to 37 C.F.R. §§ 1.56 and 1.97(c), Applicants bring to the attention ofthe
`
`Examiner the documentsonthe attachedlisting. This Information Disclosure Statementis being
`
`: filed after the events recited in Section 1.97(b) but, to the undersigned's knowledge, before the
`| mailing date of either a Final action, Quayle action, or a Notice ofAllowance. Under the
`
`provisions of 37 C.F.R. § 1.97(c), the Commissioner is hereby authorized to charge the fee of
`
`$180.00 to Deposit Account No. 06-0916 as specified by Section 1.17(p).
`
`Copies of the listed non-patentliterature documents are attached. Copies of the U.S.
`
`patents and patent publications are not enclosed.
`
`Applicants respectfully request that the Examiner consider the listed documents and
`
`indicate that they were considered by making appropriate notations on the attached form.
`
`Ex. 1004, Page 541
`
`Ex. 1004, Page 541
`
`
`
`This submission does not represent that a search has been madeorthat no better art exists
`
`and doesnot constitute an admission that eachorall of the listed documents are material or
`
`constitute “priorart." Ifthe Examinerapplies any ofthe documents asprior art against any
`
`claims in the application and Applicants determine that the cited documents do not constitute
`
`"prior art" under United States law, Applicants reserve the right to presentto the office the
`
`relevant facts and law regarding the appropriate status of such documents.
`
`Applicants further reserve the right to take appropriate action to establish the patentability
`
`of the disclosed invention over the listed documents, should one or more of the documents be
`
`applied against the claims ofthe present application.
`If there is any fee due in connection with the filing of this Statement, please charge the
`
`fee to our Deposit Account No. 06-0916.
`
`Respectfully submitted,
`
`FINNEGAN, HENDERSON, FARABOW,
`GARRETT &
`
`ER, L.L.P. Dated: March 2, 2006
`
`
`By:
`
`y
`Reg. No. 41,008
`
`Ex. 1004, Page 542
`
`Ex. 1004, Page 542
`
`
`
`IDS Form PTO/SB/08: Substitute for form 1449A/PTO
`
`EXPRESS MAIL NO. EV 860819695 US
`
`Complete if Known
`
`Application Number
`Filing Date
`First Named Inventor
`
`10/954,182
`October 1, 2004
`Hongmei ZHANG
`
`
`
`
`
`‘STATEMENT BY APPLICANTpAdUnt___ifagg
`
`ESTRADA,Michelle
`Examiner Name
`(Use as many sheets as necessary)
`wy
`
`
`og@t7TtCCT~~]~~~_|Attomey Docket Number_|9140,0016-01
`
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` U.S. PATENTS AND PUBLISHEDU.S. PATENT APPLICATIONS .
`
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`Examiner
`Cite
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`MM-DD-YYYY
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`
`FT WO 2004/106581 A2 12-09-2004|Symmorphix,Inc.
`
`FT WO 2004/106582 A2
`~
`|12-09-2004
`|Symmorphix, Inc.
`
`
`
`
`Foreign Patent Document
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`Initials”
`
`Cite
`No.!
`
`Include nameofthe author (in CAPITAL LETTERS),title of the article (when appropriate),title of the item (book,
`magazine,journal, serial, symposium,catalog, etc.), date, page(s), volume-issue number(s), publisher, city and/or
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`Translation®
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`NON PATENT LITERATURE DOCUMENTS
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`Examiner
`Signature
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`Date
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`
`EXAMINER: Initial if reference considered, whether or not citation is in conformance with MPEP 609. Drawline through
`citation if not in conformance and not considered. Include copyof this form with next communication to applicant.
`
`Ex. 1004, Page 543
`
`
`
`2 J
`: I
`3
`: J
`
`: J
`
`JC
`
`
`
`Gq
`
`aia
`
`T
`TT
`
`
`ee
`
`Note: Submission of copies of U.S. Patents and published U.S, Patent Applications is notrequired.
`
`
`
`
`
` Examiner
`
`Ex. 1004, Page 543
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`
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`IDS Form PTO/SB/08: Substitute for form 1449A/PTO
`
`INFORMATION DISCLOSURE
`STATEMENT BY APPLICANT
`
`(Use as many sheets as necessary)
`
`[Sheet{2ts
`
`EXPRESS MAIL NO. EV 860819695 US
`
`Complete if Known
`10/954, 182
`October1, 2004
`
`Application Number
`Filing Date
`
`Art Unit
`
`2823
`p2e23
`ESTRADA,Michelle _
`9140.0016-01
`
`:
`
`:
`
`
`
`Attorney Docket Number
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`Docket No. 09140.0030-01).
`
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`pf International Preliminary Examination Report mailed on April 15, 2004 in PCT/US03/24809
`
`(Attorney Docket No. 09140-0025-00304).
`Office Action issued on December 2, 2005 in U.S. Application No. 10/789,953 (Attorney
`Docket No. 09140.0030-00).
`Specification and Preliminary Amendmentasfiled for U.S. Appl. No. 11/297,057 (Attorney
`
`Response to Office Action filed January 19, 2006 in U.S. Application No. 10/851,542
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`(Attorney Docket No. 09140.0033-00).
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`NON PATENT LITERATURE DOCUMENTS
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`KIM,H-K.and YOON,Y., “Characteristics of rapid-thermal-annealed LiCoO, cathode film
`for an all-solid-state thin film microbattery,” J. Vac. Sci. Technol. A 22(4):1182-1187 (2004).
`Response to Office Action filed on October 17, 2005 in U.S. Application No. 10/291,179
`(Attorney Docket No. 09140-0001-00).
`Final Office Action issued on December 14, 2005 in U.S. Application No. 10/291,179
`(Attorney Docket No. 09140-0001-00).
`PCTInvitation to Pay Additional Fees for PCT/US01/22750, dated March 13, 2002 (Attorney
`Docket No. 09140.0002-00304).
`PCTInternational Search Report for PCT/USO1/22750, dated July 19, 2002 (Attorney Docket
`No. 09140.0002-00304).
`PCT Written Opinion for PCT/US01/22750, dated July 23, 2002 (Attorney Docket No.
`09140.0002-00304).
`PCTInternational Preliminary Examination Report for PCT/USO1/22750, dated October8,
`2002 (Attorney Docket No. 09140.0002-00304).
`Amendment/RCEfiled on March 10, 2005 in U.S. Application No. 09/903,081 (Attorney
`Docket No. 09140-0014-00)..
`Office Action issued on November28, 2005 in U.S. Application No. 09/903,081 (Attorney
`Docket No. 09140-0014-00).
`Response to Office Action filed February 17, 2006 in U.S. Application No. 11/100,856
`(Attorney Docket No. 09.140.0015-01).
`Response to Office Action filed December 5, 2005, in U.S. Application No. 10/101,863
`(Attorney Docket No. 09140.0016-00).
`Final Office Action issued on February 14, 2006, in U.S. Application No. 10/101,863
`(Attorney Docket No. 09140.0016-00).
`Response to Office Action filed February 24, 2006, in U.S. Application No, 10/101,863
`(Attorney Docket No. 09140.0016-00).
`Response to Office Action filed on November8, 2005, in U.S. Application No. 10/101,341
`(Attorney Docket No. 09140-0017-00).
`Office Action issued on February 13, 2006, in U.S. Application No. 10/101,341 (Attorney
`Docket No. 09140-0017-00).
`Response to Office Action filed on January 3, 2006 in U.S. Application No. 10/650,461
`(Attorney Docket No. 09140-0025-00).
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`Examiner
`Signature
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`“|
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`Date
`Considered
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`EXAMINER: Initial if reference considered, whetheror notcitation is in conformance with MPEP 609. Drawline through
`citation if not in conformance and not considered.
`Include copyof this form with next communication to applicant.
`
`Ex. 1004, Page 544
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`Ex. 1004, Page 544
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`EXPRESS MAIL NO. EV 860819695 US
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`Complete if Known
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`IDS Form PTO/SB/08: Substitute for form 1449A/PTO
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`10/954, 182
`
`October
`INFORMATION DISCLOSURE
`October 1, 2004
`
`ongmei
`
`
`
`
`rong
`STATEMENTBY APPLICANT
`ESTRADA,Michelle
`(Use as many sheets as necessary)
`
`Attorney Docket Number__|9140.0016-01
`
`Application Number
`Fiing Date___
`Filing Date
`Pisin
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`12008
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`
`
`NON PATENT LITERATURE DOCUMENTS
`PCT International Search Report and Written Opinion for Application No.
`PCT/US2004/014524 dated March 2, 2005 (Attorney Docket No. 09140.0033-00304).
`
`°
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`2005 (Attorney Docket No. 09140.0034-00304).
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`;
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`PCT International Preliminary Report onPatentability for Application No. PCT/US2004/014524, dated December 8, 2005 (Attorney Docket No. 09140.0033-00304). p
`
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`(|ieneencom|
`|earnras
`(Attorney Docket No. 09140.0034-00304). PCTInternational Preliminary Report on Patentability for Application No.
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`PCT/US2004/014523, dated December8, 2005 (Attorney Docket No. 09140.0034-00304).
`
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`FT| Specificationas filed for U.S. Appl. No. 11/297,057 (Attorney Docket No. 09140.0042-00). P|
`
`Examiner
`Signature
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`Date
`Considered
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`EXAMINER: Initial if reference considered, whether or not citation is in conformance with MPEP 609. Drawline through
`citation if not in conformance and not considered.
`Include copy of this form with next communication to applicant.
`Ex. 1004, Page 545
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`Ex. 1004, Page 545
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`—s
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`(12) INTERNATIONAL APPLICATION PUBLISHED UNDER THEPATENT COOPERATION TREATY (PCT)
`
`(19) World Intellectual Property
`Organization —
`Intemational Bureau
`
` - EN800000
`
`(10) International Publication Number
`(43) International Publication Date
`WO 2004/106581 A2
`9 December 2004 (09.12.2004)
`
`(81) Designated States (unless otherwise indicated, for every
`(51) International Patent Classification’:
`C23C 14/08,
`kind ofnational protection available): AE, AG, AL, AM,
`14/34
`AT, AU, AZ, BA, BB, BG, BR, BW. BY, BZ, CA, CH, CN,
`CO, CR, CU, CZ, DE, DK, DM, DZ, EC, EE, EG,ES,FI,
`GB, GD, GE, GH, GM,HR, HU, ID,IL, IN, IS, JP, KE,
`KG,KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MA, MD,
`MG, MK, MN, MW, MX, MZ, NA, NI, NO, NZ, OM, PG,
`(22) International Filing Date:—21 May 2004 (21.05.2004)
`PH,PL, PT, RO, RU, SC, SD, SE, SG, SK, SL, SY, TJ, T™,
`TN,TR, TT, TZ, UA, UG, US, UZ, VC, VN, YU, ZA, ZM,
`zw.
`
`(21) International Application Number:
`PCT/US2004/014523
`
`¥
`
`(25) Filing Language:
`
`English
`
`(26) Publication Language:
`
`English
`
`(30) Priority Data:
`60/473,379
`
`23 May 2003 (23.05.2003) US
`
`(71) Applicant (for all designated States except US): SYM-
`MORPHIX, INC. [US/US]; 1278 Reamwood Avenue,
`Sunnyvale, CA 94089-2233 (US).
`
`(84) Designated States (unless otherwise indicated, for every
`kind of regional protection available): ARIPO (BW, GH,
`GM, KE, LS, MW, MZ, NA, SD, SL, SZ, TZ, UG, ZM,
`ZW), Eurasian (AM, AZ, BY, KG, KZ, MD, RU, TJ, T™),
`European(AT, BE, BG, CH, CY, CZ, DE, DK, EE, ES,Fl,
`FR, GB, GR, HU,IE, IT, LU, MC, NL,PL, PT, RO, SE, SI,
`SK, TR), OAPI (BF, BJ, CF, CG, CI, CM, GA, GN, GQ,
`GW, ML, MR, NE, SN, TD, TG).
`
`(72) Inventors; and
`
`(75) Inventors/Applicants (for US only):|DEMARAY,
`Published:
`Richard, Ernest [US/US]; 190 Fawn Lane,Portola Valley,
`— without intemational search report and to be republished
`CA 94028 (US). NARASIMHAN, Mukundan [IN/US];
`upon receipt of that report
`293 Bluefield Drive, San Jose, CA 91536 (US).
`
`41.6581AMUU00008
`
`(74) Agent: GARRETT, Arthur, S., Finnegan, Henderson,
`Farabow, Garrett & Dunner, L.L.P., 1300 I Street N.W.,
`Washinton, D.C. 20005-3315 (US).
`
`For two-letter codes and other abbreviations, refer to the “Guid-
`ance Notes on Codes and Abbreviations” appearing at the begin-
`ning ofeach regularissue ofthe PCT Gazette.
`
`o
`
`nn
`(54) Title: TRANSPARENT CONDUCTIVE OXIDES
`
`(57) Abstract: A method of deposition ofa transparent conductive film from a metallic target is presented. A method of forming a
`oS
`&} transparent conductive oxide film according to embodiments of the present invention include depositing the transparent conductive
`(NI oxide film in a pulsed DC reactive ion process with substrate bias, and controlling at least one process parameterto affect at least one
`characteristic of the conductive oxide film. The resulting transparent oxide film, which in some embodiments can be an indium-tin
`oxide film, can exhibit a wide range of material properties depending on variations in process parameters. For example. varying the
`process parameters can result ina filmwith a wide rangeofresistive properties and surface smoothness of the film.
`
`©5
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`Transparent Conductive Oxides
`Related Applications
`The present application claims priority to U.S. Provisional Application
`[0001]
`60/473,379,“Transparent Conductive Oxides from a Metallic Target,” by R. Emest
`Demaray and Mukundan Narasimhan, filed on May 23, 2003,herein incorporated by
`referencein its entirety.
`,
`
`Background
`
`1
`
`.
`
`.
`
`
`1, Field of the Invention
`[0002]
`Thepresentinventionis related to deposition ofoxides ona substrate and,
`in particular, deposition oftransparent conductive oxides.
`
`2. Discussion of Related Art
`[0003]
`Transparent conductive oxides have awide variety ofuses, including
`applications to solar cells, organic light emitting diodes (OLEDs),electric field
`devices, current devices(i.e. touch screens),energy efficient windows, conductive
`anti-reflective devices, electromagnetic interference shields, heaters, transparent
`electrodes, coatings for cathode ray tube (CRT) displays, to name only a few.
`Another important application is for touch sensitive MEMSdevices, such as those
`used, for example, in fingerprint sensors and such. In many cases, the electrical
`properties ofthe conductingfilm is ofgreat importance.
`[0004]
`Specifically, for OLED applications,films deposited with current
`technologiesare generally rough, resultingin stress risers and field concentration
`issues, that can cause leakage. Further, asperities in the resulting film can induce
`lifetime dependent defects in nearest neighborfilms that can shorten device lifetimes.
`Additionally, the brightness ofthe emergent light from the OLED can be reduced.
`{0005}
`Transparent conductive oxides have been deposited from ceramic targets
`by RF magnetronsputtering. However, the surface ofproperties ofthe resulting films
`often include nodules or asperites which can cause arcing, defects, surface roughness,
`_ and other deleterious effects in the resulting film. Additionally, ceramic targets tend
`to be moreexpensive to produce than metallic targets.
`[0006]
`Previousattempts at deposition oftransparent conductive oxides, for
`example indium tin oxide (ITO), with metallic targets have presented numerous
`
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`problems, including small process windows, problems in process controllability, a
`disappearing anodeeffect, and particle deposition on the film. Suchattempts have
`been abandoned. Deposition with ceramic targets has also been difficult, including
`problems with particles, nodule formation, and arching during deposition. In both
`cases, film smoothness has presented major difficulties. Additionally, control offilm
`parameters such as, for example,resistivity and transparency has been difficult.
`[0007]
`Therefore, there is need for cost effective deposition of smoother layers of
`
`transparent conductive oxides with greater control over layer properties such as
`
`resistivity and transparency.
`
`Summary
`In accordance with the present invention, a method of depositing of a
`[0008]
`transparent conductive film from a metallic target is presented. A methodofforming
`a transparent conductive oxide film according to embodiments ofthe present
`invention includes depositing the transparent conductive oxide film in a pulsed DC
`reactive ion process with substrate bias, and controlling at least one process parameter
`to provide at least one characteristic ofthe conductive oxide film at a particular value.
`[0009]
`A method ofdepositing a transparent conductive oxide film on a substrate
`according to some embodiments of the invention, then, includes placing the substrate
`
`in a reaction chamber, adjusting power to a pulsed DC power supply coupled to a
`target in the reaction chamber, adjusting an RF bias power coupled to the substrate,
`adjusting gas flow into the reaction chamber, and providing a magneticfield at the
`target in order to direct deposition of the transparent conductive oxide film on the
`substrate in a pulsed-dc biased reactive-ion deposition process, wherein the
`transparent conductive oxide film has a particular characteristic.
`[0010]=Theresulting transparent oxide film, which can be deposited according to
`some embodiments ofthe present invention, can be an indium-tin oxide (ITO)film.
`An ITO film can have a wide range of material properties depending on variations in
`process parameters. For example, varying the process parameters according to some
`embodiments ofthe present invention can result in a wide rangeofresistive properties
`and surface smoothnessofthe film.
`
`[0011]§These and other embodiments of the invention are further discussed below
`
`2
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`with reference to the following figures.
`Short Description of the Figures
`Figures 1A and1Billustrate a pulsed-DC biased reactive ion deposition |
`[0012]
`apparatus that can beutilized in the methods of depositing accordingto the present
`invention.
`|
`.
`[0013]
`Figure 2 shows an exampleofa target that can be utilized in the reactor
`illustrated in Figures 1A and 1B
`j0014]
`Figure 3A shows an Atomic Force Microscopy (AFM) iimageofan
`indium-tin-oxide (ITO)process accordingto some embodiments ofthe present
`
`invention.
`Figure 3B shows an Atomic Force Microscopy (AFM) image ofanother
`[0015]
`ITO process deposited using a process according to some embodiments ofthe present
`invention.
`.
`[0016]
`Figure 4 shows the variation of bulk resistivity of an ITO layer according
`to some embodiments ofthe present invention as a function ofthe oxygen flow for
`two different target powers before and after a 250°C anneal in vacuum.
`[0017]
`Figure 5shows the variation ofthe sheet resistance of anITO layer
`according to some embodiments ofthe present invention as a function ofthe oxygen
`flow used for two different target powers before and after a 250 °C anneal in vacuum.
`[0018}
`Figure 6 shows thetarget current and voltage (min and max)as afunction
`ofoxygenflow.
`,
`[0019]
`Figure 7 shows the thickness changein layers ofITO according to
`embodiments ofthe present invention as a function of oxygen flow.
`[0020]
`Figure 8 illustratesthe relationship between oxygen flow and oxygen
`|
`partial pressure for a metallic target.
`[0021]
`Figures 9A-9Dillustrate the smoothness oftransparent conductive oxides
`deposited with ceramic targets according to the present invention.
`.
`[0022]
`In the figures, elements having the same designation have the sameor
`similar function.
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`Detailed Description
`Deposition of materials by pulsed-DC biased reactive ion deposition is
`[0023]
`describedin U.S. Patent Application Serial No. 10/101863, entitled “Biased Pulse DC
`Reactive Sputtering ofOxide Films,”to HongmeiZhang, et al., filed on March 16,
`2002. Preparation oftargets is described in U.S. Patent Application Serial No.
`10/101,341,entitled “Rare-Earth Pre-Alloyed PVD Targets for Dielectric Planar
`Applications,”to Vassiliki Milonopoulou,et al., filed on March 16, 2002. U.S. Patent
`‘Application Serial No. 10/101863 and U.S. Patent Application Serial No. 10/101,341
`are each assigned to the same assignee as is the present disclosure and each is
`incorporated herein in their entirety. Deposition of oxide materials has also been
`described in U.S. Patent No. 6,506,289, which is also herein incorporated by reference
`in its entirety. Transparent oxidefilms are deposited utilizing processes similar to
`those specifically described in U.S. Patent No. 6,506,289 and U.S. Application Serial _
`No.10/101863.
`|
`|
`[0024] Figure 1A shows a schematic ofa reactor apparatus 10 for sputtering material
`fromatarget 12 accordingto the present invention. In some embodiments, apparatus
`10 may,for example, be adapted from an AKT-1600 PVD (400 X 500 mm substrate
`size) system from Applied Komatsu or an AKT-4300 (600 X 720 mm substratesize)
`systemfrom Applied Komatsu, Santa Clara, CA. The AKT-1600 reactor, for
`example, has three deposition chambers connected by a vacuum transport chamber.
`These Komatsu reactors can be modified such that pulsed DC power is supplied to the
`target and RF poweris supplied to the substrate during deposition of a material film.
`[0025] Apparatus 10 includes target 12 whichis electrically coupled throughafilter
`15 to a pulsed DC power supply 14. In some embodiments, target 12 is a wide area
`sputter sourcetarget, which provides material to be deposited on a substrate 16.
`Substrate 16 is positioned parallel to and opposite target 12. Target 12 functions as a
`cathode when power is applied to it and is equivalently termed a cathode. Application
`ofpowerto target 12 creates a plasma 53. Substrate 16 is capacitively coupled to an
`electrode 17 through an insulator 54. Electrode 17 can be coupled to an RF power
`supply 18. A magnet 20is scanned acrossthe top of target 12.
`[0026] For pulsed reactive dc magnetron sputtering, as performed by apparatus 10,
`
`4
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`the polarity ofthe power supplied to target 12 by power supply 14 oscillates between
`negative and positive potentials. During the positive period, the insulating layer on
`the surface oftarget 12 is discharged and arcing is prevented. To obtain arcfree
`deposition, the pulsing frequency exceeds a critical frequency that can depend on
`target material, cathode current and reverse time. High quality oxide films can be
`made using reactive pulse DC magnetron sputtering as shown in apparatus 10.
`_ [0027] Pulsed DC power supply 14 can be any pulsed DC powersupply, for example
`an AE Pinnacle plus 10K. by Advanced Energy, Inc. With this DC power supply, up
`to 10 kW of pulsed DC power can be supplied at a frequency of between 0 and 350
`KHz. Thereverse voltage can be 10% ofthe negative target voltage. Utilization of
`other power supplies can lead to different power characteristics, frequency
`characteristics and reverse voltage percentages. The reverse time on this embodiment
`ofpower supply 14 can be adjusted between 0 and 5 pss.
`[0028] Filter 15 prevents the bias power from power supply 18 from coupling into
`pulsed DC powersupply 14. In some embodiments, power supply 18 can be a2 MHz
`RF power supply, for example aNova-25 power supply made by ENI, Colorado
`Springs, Co.
`[0029] In some embodiments,filter 15 can be a 2 MHz sinusoidal band rejection
`filter. In some embodiments, the band width ofthe filter can be approximately 100
`kHz, Filter 15, therefore, prevents the 2 MHz power from t