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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 9 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 10 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 11 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 12 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 13 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 14 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 15 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 17 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 18 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 19 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 20 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 21 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 22 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 23 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 24 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 25 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 28 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 29 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 30 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 31 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 33 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 34 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 35 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 36 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 37 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 38 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 39 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 40 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 41 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 42 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 43 of 4121
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 44 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 45 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 46 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 47 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 48 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 49 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 50 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 51 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 52 of 412
`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 52 of 412
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`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 53 of 412
`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 53 of 412
`
`ce>) Papas:Pant ATE
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`European Patent Office
`Office européen des brevets
`
`(11)
`
`EP 0 652 308 A3
`
`(12)
`
`EUROPEANPATENT APPLICATION
`
`(88) Date of publication A3:
`17.12.1997 Bulletin 1997/51
`
`(43) Date of publication A2:
`10.05.1995 Bulletin 1995/19
`
`(21) Application number: 94116188.7
`
`(22) Dateof filing: 13.10.1994
`
`(84) Designated Contracting States:
`DE FR GB NL
`
`(30) Priority: 14.10.1993 JP 281748/93
`20.10.1993 JP 285674/93
`10.12.1993 JP 341281/93
`29.03.1994 JP 58887/94
`
`.
`(71) Applicants:
`* NEURALSYSTEMS CORPORATION
`Tokyo-to (JP)
`» MEGA CHIPS CORPORATION
`Suita-shi, Osaka-fu (JP)
`
`(72) Inventors:
`* Asakawa,Toshifumi
`Yamato-shi, Kanagawa-ken (JP)
`
`(51) Int. cl.®: C30B 23/02
`
`« Shindo, Masahiro,
`c/o Mega Chips Corporation
`Suita-shi, Osaka-fu (JP)
`¢ Yoshimizu, Toshikazu,
`c/o Mega Chips Corporation
`Suita-shi, Osaka-tu (JP)
`» Ueyama, Sumiyoshi,
`c/o Mega Chips Corporation
`Suita-shi, Osaka-fu (JP)
`
`(74) Representative:
`KUHNEN, WACKER & PARTNER
`Alois-Steinecker-Strasse 22
`85354 Freising (DE)
`
`
`
`(54) Method of and apparatus for forming single-crystalline thin film
`
`In order to form a single-crystalline thin film on
`(57)
`a polycrystalline substrate using plasma CVD, a down-
`wardly directed mainly neutral Ne atom current
`is
`formed by an ECRion generator (2). A reaction gas
`suchas silane gas which is supplied from a reaction gas
`inlet pipe (13) is sprayed onto an SiOz substrate (11) by
`an action of the Ne atom current, so that an amorphous
`Si thin film is grown on the substrate (11) by a plasma
`CVD reaction. At the sametime, a part of the Ne atom
`current having high directivity is directly incident upon
`the substrate (11), while another part thereof is incident
`upon the substrate (11) after its course is bent by a
`reflector (12). The reflector (12) is so set that all direc-
`tions of the parts of the Ne atom current which areinci-
`dent upon the substrate (11) are perpendicular to
`densest planes of single-crystalline Si. Therefore, the
`as-grown amorphous Si is sequentially converted to a
`single-crystalline Si thin film having crystal axes which
`are so regulated that the densest planes are oriented
`perpendicularly to the respective directions of
`inci-
`dence,by an action of the law of Bravais. Thus,a single-
`crystalline thin film is formed on a polycrystalline sub-
`strate.
`
`FIG. 13
`
`
`
`Printed by Xerax (UK) Business Services
`2.18.43.4
`
`EP0652308A3
`
`

`

`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 54 of 412
`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 54 of 412
`
`(
`
`came
`
`)) EuropeanPatent =
`
`Office
`
`WROPEANSEARCHREPORT
`
`ApplicationNumber
`
`EP 94 11 6188
`
`of relevant passage 3
`
`PATENT ABSTRACTS OF JAPAN
`vol. 10, no. 107 (C-341), 22 April 1986
`& JP 60 235788 A
`(HITACHI SEISAKUSHO KK),
`22 November 1985,
`* abstract *
`
`Relevant
`to claim
`
`CLASSIFICATION OF THE
`APPLICATION (IntCl.6)
`
`C30B23/02
`
`.
`
`PATENT ABSTRACTS OF JAPAN
`
`:
`
`(P04001) . Citation of document with indication, where appropriate,
`
`vol. 914, no. 543 (C-0783), 30 November
`1990
`& JP 02 229792 A
`(NIYUURARU SYST:KK), 12
`September 1990,
`* abstract *
`
`PATENT ABSTRACTS OF JAPAN
`vol. 095, no. 003, 28 April 1995
`& JP 06 340500 A
`(NIYUURARU SYST:KK), 13
`December 1994,
`*DOCUMENT WHICH MAY THROW DOUBT ON THE
`PRIORITY CLAIMED*
`* abstract * a
`
`/
`
`:
`
`. TECHNICAL FIELDS
`
`C30B
`
`.
`
`Place of search
`THE HAGUE
`CATEGORY OF CITED DOCUMENTS
`
`X: particularly relevant # taken alone
`Y : partioularly relevant # combined with another
`document of the same catagory
`O : non-written disclosure
`P;
`
`
`
`EPOFORM150303.62
`
`Exarniner
`Oate of completion of the search
`Gregg, N
`17 October 1997
`T : theory or principle undertying the
`€: earlier patent document, but published on, or
`efter the filing date
`: doournent oited in the
`D:
`L : dooument cited for other reasons
`& : member of the same patent family, corresponding
`document
`
`

`

` eS
`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 55 of 412
`5°20-cv-0934
`
`Patent Abstracts of Japan
`
`yf PUBLICATION NUMBER
`PUBLICATION DATE
`
`APPLICATION DATE
`APPLICATION NUMBER
`
`:
`:
`
`:
`:
`
`07233469
`05-09-95
`
`22-02-94 -
`06024420
`
`APPLICANT : ASAHI GLASS CO LTD;
`
`INVENTOR
`
`SASAKI KENICHI;
`
`INT.CL.
`
`C23C 14/34 CO4B 35/46 C23C 14/08
`
`TITLE
`
`TARGET, ITS PRODUCTION AND PRODUCTION OF HIGH-REFRACTIVE-INDEX FILM
`
`ABSTRACT
`
`PURPOSE: To produce a highly productive oxide sintered compact for a sputtering target
`having a low resistivity and a high content of oxygen by hot-pressing titanium dioxide
`powderin a nonoxidizing atmosphere and sintering the compact.
`
`CONSTITUTION: The powderoftitanium dioxide having 0.05-40um grain diameteris
`hot-pressed at 1000-1300°C and 50-100kg/cm?in a nonoxidizing
`atmosphereofAr, etc., to obtain an oxide sintered compact consisting essentially of TiO,
`(1<x<2). A sputtering target having <10Qcm resistivity at room temp. and contg.
`235wt.% oxygen is formed from the sintered compact. A metal oxide other than TiO, is
`incorporated, as required, into the target by <50%. The oxide of at least one kind among
`Cr, Ce, Zr, Y, Nb, Ta, Si, Al and B is preferably used for the metal oxide. DC sputtering is
`conducted by using the target to form a high-refractive-index uniform transparentfilm at a
`high rate.
`
`COPYRIGHT:(C)1995,JPO
`
`NSDOCID: <JP___407233463A_AJ_>
`
`

`

`INTERNATIONAL APPLICATION PUBLISHED UNDER THE PATENT COOPERATION TREATY (PCT)
`(51) International Patent Classification 7 :
`C03C 13/04, HOS 3/06
`
`(11) International Publication Number:
`
`WO 00/21898
`
`(43) International Publication Date:
`
`20 April 2000 (20.04.00)
`
`(21) International Application Number:
`
`PCT/KR99/00609
`
`(22) International Filing Date:
`
`11 October 1999 (11.10.99)
`
`(81) Designated States: AU, CA, CN, JP, RU, European patent
`(AT, BE, CH, CY, DE, DK,ES, FI, FR, GB, GR,JE, IT,
`LU, MC, NL,PT, SE).
`
`(30) Priority Data:
`1998/42713
`
`13 October 1998 (13.10.98)
`
`KR
`
`(71) Applicant: SAMSUNG ELECTRONICS CO., LTD. [KR/KR};
`416, Maetan-dong, Paldal-gu, Suwon-city, Kyunggi-do
`442-373 (KR).
`
`Published
`With international search report.
`Before the expiration of the time limit for amending the
`claims and to be republished in the event of the receipt of
`amendments.
`
`(74) Agent: LEE, Young-pil; The Cheonghwa Building, 1571-18,
`Seocho-dong, Seocho-gu, Seoul 137-073 (KR).
`
`(54) Title: OPTICAL FIBER FOR LIGHT AMPLIFIER
`
`(57) Abstract
`
`Anoptical fiber used for an optical amplifier, which is formed by doping glass with rare-earth ions. Both praseodymium ions (Pr*3)
`and erbium ions (Ert3) are used as the rare-earth ions, and the glass is a fluoride glass or a sulfide glass. The optical fiber can be used
`at both wavelengths of 1.3 4m and 1.55 zm. The light amplification efficiency of an optical amplifier made of the optical fiber can be
`
`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 56 of 412
`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 56 of 412
`
`PCT
`
`WORLD INTELLECTUAL PROPERTY ORGANIZATION
`Intemational Bureau
`
`
`
`(72) Inventors: HEO, Jong; 8-401, Kyosoo Apt., Jigok-dong,
`Nam-gu, Pohang-city, Kyungsangbuk-do 790-390 (KR).
`LEE, Dong~chin; 7/1, 94-10, Onchun |—dong, Tongrae~gu,
`Pusan 607-061 (KR). PARK, Se-ho; 246-55, Junggok
`i-dong, Kwangjin-gu, Seoul 143-221 (KR).
`JUNG,
`Sun-tae; 602-1503, Taeyoung Apt., 1075, Hogae-dong,
`Tongan-gu, Anyang-city, Kyungki-do 431-080 (KR).
`KIM, Hyoun-soo; 801-1002 Jinheung Apt., Imae-dong,
`Bundang-gu, Sungnam-city, Kyungki-do 463-060 (KR).
`
`improved compared to an optical amplifier formed of only Pr*3 or only Er*3,
`
`

`

`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 57 of 412
`
`Codes used to identify States party to the PCT on the front pages of pamphlets publishing international applications under the PCT.
`
`FOR THE PURPOSES OF INFORMATION ONLY
`
`AL
`AM
`AT
`AU
`AZ
`BA
`BB
`BE
`BF
`BG
`BJ
`BR
`BY
`CA
`CF
`CG
`CH
`Cl
`CM
`CN
`cu
`CZ
`DE
`DK
`EE
`
`Albania
`Annenia
`Austria
`Australia
`Azerbaijan
`Bosnia and Herzegovina
`Barbados
`Belgium
`Burkina Paso
`Bulgaria
`Benin
`Brazil
`Belarus
`Canada
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`Congo
`Switzerland
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`China
`Cuba
`Czech Republic
`Germany
`Denmark
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`
`ES
`FI
`•'R
`GA
`GB
`GE
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`HU
`IE
`IL
`IS
`IT
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`KE
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`
`KR
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`u
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`LR
`
`Spain
`Finland
`France
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`United Kingdom
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`Guinea
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`!smel
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`Saint Lucia
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`
`LS
`LT
`LU
`LV
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`MK
`
`ML
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`MX
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`NL
`NO
`NZ
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`RO
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`SG
`
`Lesotho
`Lithuania
`Luxembourg
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`The former Yugoslav
`Republic of Macedonia
`Mali
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`Mexico
`Niger
`Netherlands
`Norway
`New Zealand
`Poland
`Ponugal
`Romania
`Russian Federation
`Sudan
`Sweden
`Singapore
`
`SI
`SK
`SN
`sz
`TD
`TG
`TJ
`TM
`TR
`TT
`UA
`UG
`us
`uz
`VN
`YU
`zw
`
`Slovenia
`Slovakia
`Senegal
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`Chad
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`Turkey
`Trinidad and Tobago
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`Viet Nam
`Yugoslavia
`Zimbabwe
`
`

`

`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 58 of 412
`
`W000/21898
`
`PCT/KR99/00609
`
`1
`
`OPTICAL FIBER FOR LIGHT AMPLIFIER
`
`Technical Field
`
`The present invention relates to optical fibers for use in a light amplifier,
`
`5 and more particularly, to an optical fiber for use in a light amplifier which can
`
`be used at wavelengths of both 1.3 µm and 1.55 µm.
`
`Background Art
`
`The wavelength of light used in optical communications has been
`
`10
`
`shifted from a wavelength of 1.3 µm to a wavelength of 1.55 µm. In general,
`
`praseodymium ions {Pr+~ which are used to dope an optical fiber, are used to
`amplify an optical signal having a wavelength of 1.3 µm while erbium ion (Er+3
`which are used to dope an optical fiber, are used to amplify an optical signal
`
`)
`
`having a wavelength of 1.55 µm.
`
`15
`
`U.S. Patent No. 5,486,947 discloses an optical fiber for use in an optical
`
`amplifier, which are capable of operating with optical sufficient optical gain at
`the 1.3 µm wavelength. The optical fiber is a fluoride glass optical fiber
`
`containing rare earth metal ions in a core glass, wherein the refractive index
`
`20
`
`difference between the core and a cladding layer is above 1.4%, and the glass
`contains lead difluoride (PbF J in a proportion of 25 mol % or less based on the
`total composition for forming the glass.
`
`Now, both wavelengths of 1.3 µm and 1.55 µm are used in many optical
`
`communications related fields. Thus, different parts which are suitable for
`
`each wavelength, are required to construct an optical circuit, so that
`
`25 development cost increases in addition to switching cost for switching the
`
`wavelengths.
`
`Disclosure of the Invention
`
`An object of the present invention is to provide an optical fiber for use
`
`30
`
`in an optical amplifier, which can be used for both the 1.3 µm and 1.55 µm
`
`bands.
`
`

`

`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 59 of 412
`
`W000/21898
`
`PCT/KR99/00609
`
`2
`
`According to an aspect of the present invention, there is provided an
`
`5
`
`) are
`
`optical fiber for an optical amplifier, which is formed by doping glass with rare(cid:173)
`) and erbium ions (Er+3
`earth ions, wherein both praseodymium ions (Pt3
`used as the rare-earth ions, and the glass is a fluoride glass or a sulfide glass.
`Preferably, the content of Pr+3 is 100-1000 ppm and the content of Er+3
`is 100-5000 ppm. If the Pr+3 and Er+3 content is outside the above range, light
`amplification efficiency is undesirably lowered. Also, the mixing ratio of Pr+3 to
`If the ratio of Pr+3 to Er+3
`Er+3
`, by weight, may be between 1: 1 and 1 :3.
`exceeds the above ratio, fluorescence emission quantity at the wavelength of
`IO 1.55 µm is decreased. Conversely, if the ratio of Pr+3 to Er+3 is less than the
`above ratio, the amplification at the wavelength of 1.3 µm unfavorably
`
`decreased.
`
`Brief Description of the Drawings
`
`15
`
`FIG. 1 shows the fluorescence emission spectrum at wavelengths of 1.3
`µm and 1.55 µm according to the amount of Er+3 in optical fibers, when a laser
`beam having a wavelength of 980 nm is irradiated onto an optical fiber which
`is formed by doping glass made of GeigAs8Ga1S62 with Pr+3 and Er+3
`, wherein
`the fluorescence emission at the wavelength of 1.3 µm is caused by the
`level to the 3H 5 level in Pr+3 doped
`20 electron transition of Pr+ from the 1G
`4
`fibers, and that at the wavelength of 1.55 µm is caused by the transition 411312
`... 411512 in Er+ doped fibers ;
`FIG. 2 is a graph showing the fluorescence lifetime of Pr+3 at the 1G4
`level and of Er+3 at the 411/2 level and 411/2 level according to the amount of
`25 Er+3 in optical fibers, when a laser beam having a wavelength of 980 nm is
`irradiated onto an optical fiber which is formed by doping a GeigAs8Ga1S62
`glass with Pr+3 and Er+3;
`FIG. 3 is a diagram illustrating energy transfer between Pr+3 and Er+3
`
`ions;
`
`30
`
`FIG. 4 shows the fluorescence emission spectrum at the wavelength of
`1.3 µm by the electron transition of Pr+3 from the 1G4 level to the 3H5 level
`when a laser beam having a wavelength of 1020 nm is irradiated onto an
`optical fiber which is formed by d.oping a Ge2gAs8Ga1S62 glass with Pr+3
`
`;
`
`

`

`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 60 of 412
`
`W000/21898
`
`PCT/KR99/00609
`
`3
`
`FIG. 5 shows the fluorescence emission spectrum at the wavelength of
`1.55 µm by the electron transition of Er+3 from the 411312 level to the 411512 level
`when a laser beam having a wavelength of 980 nm is irradiated onto an optical
`fiber which is formed by doping a Ge~s8Ga1S62 glass with Er+3
`FIG. 6 shows the fluorescence emission spectrum at the wavelengths
`of 1.3 µm and 1.55 µm according to the amount of Pr+3 in optical fibers, when
`
`; and
`
`a laser beam having a wavelength of 980 nm is irradiated onto an optical fiber
`which is formed by doping a Ge2gAs8Ga1S62 glass with Pr+3 and Er+3
`, wherein
`the fluorescence emission at the wavelength of 1.3 µm is due to the electron
`transition of Pr+ from the 10 4 level to the 3Hs level, and that at the wavelength
`of 1.55 µm is due to the electron transition of Er+ from the 411312 level to the
`411512 level.
`
`Best mode for carrying out the Invention
`
`The present invention provides an optical fiber for use in a light
`amplifier, which can be used at wavelengths of both 1.3 µm and 1.55 µm, by
`using a laser beam having a wavelength of 980 nm as a light source for
`exciting an optical fiber formed of Pr+3 and Er*3
`
`• In the present invention, the
`
`5
`
`10
`
`15
`
`20
`
`term "fibers" refers ro shapes with a wide range of diameters, not merely thin
`fibers. For example, a fiber may have diameter of 5 to 1 OOmm. In the present
`invention, the fiber contains Pr+3 and Er+3
`, wherein the maximum absorption
`peak of Er+3 in a laser beam having wavelength 980 nm is at the 411112 1evel.
`In this case, two ions are simultaneously excited, so that Pr+3 emits
`fluorescence at 1.3 µm and Er+3 emits fluorescence at 1.55 µm. In particular,
`25 as shown in FIG. 3, the fluorescence lifetime of Pr+3 at the 10 4
`level is
`elongated due to the energy transfer from Er+3
`, so that light amplification
`
`efficiency is improved compared to a conventional optical fiber containing only
`Pr+3•
`
`30
`
`Preferably, in the present invention, a fluoride or sulfide glass is used
`to minimize lattice vibration relaxation of Pr+3 from the 10 4 level to 3F 4 level.
`The fluoride glass may be a ZBLAN glass which is a fluoride containing
`
`zirconium (Zr), barium (Ba), lanthanum (La), aluminum (Al) and sodium (Na),
`
`and the sulfide glass may be a g.ermanium-arsenic-gallium-sulfur (Ge-As-Ga-
`
`

`

`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 61 of 412
`
`W000/21898
`
`PCTIKR99/00609
`
`4
`
`S) or Ge-As-S glass. Here, using the sulfide glass can further minimize the
`lattice vibration relaxation of Pr+3 from the 10 4 level to the 3F4 level compared
`to the case of using the fluoride glass. However, using the fluoride glass rather
`
`than a sulfide glass generally makes the manufacture of optical fiber easier.
`
`5
`
`In order to maximize the light amplification efficiency at both
`wavelengths of 1.3 µm and 1.55 µm, the mixing weight ratio of Pr+3 and Er+3 is
`adjusted to be between 1:1and1:3.
`
`Hereinafter, the present invention will be described using the following
`
`examples. However, these examples are merely illustrative and the present
`
`10
`
`invention is not limited thereto.
`
`Comparative Example 1
`
`Ge, As, Ga and S having a purity of 99.999% or more, were weighted
`in an atomic ratio of 29:8:1 :62 in a glove box where the content of hydroxy
`
`15
`
`(OH) group and oxygen was maintained to be 10 ppm or less, and Pr metal
`powder was added in amount of 300 ppm to give the Pr+3
`•
`After filling a Si02 test tube with the above composition, the test tube
`was left under a vacuum condition of 0.1 mTorr for a predetermined period of
`
`time. Then, the test tube was made airtight by sealing it with an oxy-propane
`flame.
`
`20
`
`Following this, the test tube was put into a rocking furnace such that the
`
`composition comprised in the test tube was completely mixed, and the
`
`resultant was kept at 950°C for 12 hours. Then, the test tube was quenched
`
`in air, and heated in a furnace which was set at 400°C for 1 hour. After the
`
`25 heating process, the test tube was slowly cooled to room temperature and
`broken into pieces, resulting in an optical fiber formed of a Pr+3-doped sulfide
`glass of GezA$8Ga1S62 in which the amount of lattice vibration relaxation was
`slight. The optical fiber was cut into a disc shape (having a diameter of 10 mm
`
`and a thickness of 3 mm) and polished.
`Then, the fluorescence spectrum and fluorescence lifetime of the
`
`30
`
`resultant were measured using a laser beam having a wavelength of 1017
`nm as a source of light excitation. At this wavelength, Pr•3 at the 10 4 level
`showed a maximum light absorption.
`
`

`

`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 62 of 412
`
`W000/21898
`
`PCT/KR99/00609
`
`5
`
`As a result, the fluorescence emission at a wavelength of 1.3 µm,
`which was caused by electron transition of Pr+3 from the 10 4 level to 3H5
`level, was observed (see FIG. 4), and the fluorescence lifetime was 305
`µsec (see FIG. 2).
`
`5
`
`Comparative Example 2
`
`An optical fiber was manufactured in the same manner as in
`Comparative Example 1 except that Er+3 was used instead of Pr+3
`• Er2S3
`was used as the source of Er+3
`• Then, the optical fiber was cut into a disc
`10 shape (having a diameter of 10 mm and a thickness of 3 mm) and polished.
`Then, the fluorescence spectrum and fluorescence lifetime of the resultant
`
`15
`
`were measured using a laser beam having a wavelength of 980 nm as a
`source of light excitation. At this wavelength, Er+3 at the 411112 level showed
`a maximum light absorption.
`As a result, the fluorescence emission at a wavelength of 1.55 µm,
`which was caused by electron transition of Er+3 from the 411312 level to 411512
`level, was observed (see FIG. 5), and the fluorescence lifetime at the 411112
`4113n levels was 2100 µsec and 3400 µsec, respectively (see FIG. 2)
`and
`
`20
`
`Example 1
`
`An optical fiber was manufactured in the same manner as in
`Comparative Example 1 except that Er+3 was further added in the amount of
`300 ppm together with 300 ppm of Pr•3
`
`• Then, the optical fiber was cut into
`
`a disc shape (having a diameter of 10 mm and a thickness of 3 mm) and
`
`25 polished. Then, the fluorescence spectrum and fluorescence lifetime of the
`resultant were measured using a laser beam having a wavelength of 980 nm
`as a source of light excitation. At this wavelength, Er•3 at the 4111n level
`showed a maximum light absorption.
`As a result, the fluorescence emission of Pr+3
`, which was caused by
`30 electron transition from 10 4 level to 3H5 level and that of Er+3
`, which was
`caused by electron transition from 4113n level to 411512 level were observed
`simultaneously at the wavelengths of 1.3 µm and 1.55 µm, respectively (see
`
`

`

`Case 5:20-cv-09341-EJD Document 138-10 Filed 03/18/22 Page 63 of 412
`
`W000/21898
`
`PCT/KR99/00609
`
`6
`
`FIG. 1 (a)). The intensify of fluorescence was increased at each wavelength
`
`compared to that of Comparative Examples 1-2. Also, the fluorescence
`lifetime of Pr+3 at the 10 4 level was 605 µsec, and the fluorescence lifetime
`of Er•3 at the 4111ri and 4113ri
`levels was 824 µsec and 3120 µsec,
`respectively (see FIG. 2).
`
`5
`
`According to Example 1, as shown in FIG. 3, the simultaneous
`
`fluorescence emission at the wavelengths of 1.3 µm and 1.55 µm was due
`to the effective energy transfer indicated by "b". Thus, the optical fiber
`obtained in Example 1 can be used at wavelengths of both 1.3 µm and 1.55
`
`10 µm.
`
`Also, the fluorescence lifetime of Pr•3 at the 10 4 level was markedly
`elongated to 605 µsec compared to Comparative Example 1, and the light
`amplification efficiency at the wavelength of 1.3 µm was further improved by
`adding both Pr•3 and Er•3
`• However, the fluorescence lifetime of Er •3at the 4111
`ri
`level was 3120 µsec, which is lower than in Comparative Example 2, thus
`
`15
`
`lowering light amplification efficiency. This is due to the energy transfer
`
`indicated by "e".
`
`Example 2
`
`20
`
`An optical fiber was manufactured in the same manner as in
`Comparative Example 1 except that 500 ppm of Er•3 was further added
`together with 300 ppm of Pr•3
`
`• Then, the optical fiber was cut into a disc
`
`shape (having a diameter of 10 mm and a thickness of 3 mm} and polished.
`
`Then, the fluorescence spectrum and fluorescence lifetime of the resultant
`25 were measured using a laser beam having a wavelength of 980 nm as a
`source of light excitation. At this wavelength, Et3 at the 411112 level showed
`a maximum light absorption.
`As a result, the fluorescence emission of Pr•3
`, which was caused by
`electron transition from 10 4 level to 3H5 level' and that of Er•3
`, which was
`30 caused by electron transition from 411312 level to 411512 level were observed
`simultaneously at the wavelengths of 1.3 µm and 1.55 µm, respectively (see
`FIG. 1 (b)). The intensify of fluorescence was increased at each wavelength
`
`

`

`Case 5:20-cv-09341-EJD Document 138-1