Free Redacted Document - District Court of Delaware - Delaware

Case 1:05-cv-00737-JJF

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EXHIBIT B
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Case 1:05-cv-00737-JJF Document 162-3ANDFiled 09/04/2008 Page 7 of 50 E,UNITED STATESPATENT TRADEMARKQFFICE
Docket No. C-40.121-AU Anticipated Classification of this Application: Subclass Class 526 "Express Mail" mailing ,-+-6i:;umber TB 1 ~ a t e o f D e ~ o s i t O ~ t 0 b 18, 1995 er

92922488US

18/54449\,

I hereby certify thatthis paper or fee is,being deposited with the United States Postal Service, with suificient postage "Express Mail Post Office t o Addressee3ervice under 37 CFR 1.10 on the date indicated above and isaddresied t o the om missioner of Patents and Trademarks, Washington, D.C. 20231

Stephen
ner of Patents and Trademarks

P. Krupp

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continuation ) divisional ) application under 37 CFR 1.60 and claiming benefit under 35 USC 120 of pending prior application Serial No. 08378,998 filed on January 27,1995 of Pak-Winq Steve Chum; Ronald P. Markovich; Georqe W. Kniqht; Shih-Yaw Lai for FABRICATEDARTICLES MADEFROMETHYLENE POLYMERBLENDS 1.
, 2.

This is a request for filing a

.

Enclosed isa copy o f the prior application, including the oath or declaration as originally filed. Cancel in this application original claims of the prior application before calculating the filing fee.

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~ h e f i l i f i e is calculated below. n~

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Nu ber m ' Filed Total Claims 30 -20 J lnaependent ClaiTs 4 -3 Multiple Dependent Claims Presented Total Filing Fee

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$ 22.00 = $ 78.00 = $250.00 = =
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Basic Fee $750.00 220 78

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The Commissioner is hereby authorized t o charge any fees which may be required, or credit any overpayment,_to Account No. 04-1512 Th~s sheet 1 enclosed In triplicate. s Amend thespecification by inserting after Title of the Invention: Cross-Reference t o RelatedApplication. This is a acontinuation divisional of application Serial No., 08378,998 filed January 27,1995 -

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Transfer the drawingsfrom the prior applicatlon to this application and abandon said prior appllcation as of the filing date accorded this application. Aduplicate copy of this sheet is enclosed for filing in the prior application file. (May only be used if signed by person authorized in Rule 138 and before payment of base issue fee.) ~ e drawings are enclosed. w

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The Dow Chemical Company The prior application is assigned to [7 The prior application is asslgned of recocd to Frame No. recorded at Reel No.

by vlrtue of an unrecorded assignment. and is

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The inventorship of this application is the same as that of the prior copending U.S. applicatiot~: Fewer Inventors are t o be named in this applicatlon than In the prior copending U.S. application. Delete as inventor(s) in this application. The Power of Attorney in the prior application is t o STEPHEN P. KRUPP, Req. No. 34,366; L. Wayne White, Req. NO.25,41* Glenn H. Korfhaqe, Req. No. 27,204; Richard G. Waterman, Reg. No. 20,128 Please address all communicationst o Osborne K. McKinney, 2301 Brazosport Blvd., 8-1211; Freeport,Texas 77541. 3 a ! The power appears in the original papers in the prior application: ~ b . 0 The power does not appear in the origlnal papers. Acopy of the power in the prior application isenclosed. c. Recognize as Associate Attorney Osborne K. McKinney whose and whose phone number is 1 4 0 9 ) 238-7889 Registration No. is P-40,084

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11.

A Preliminary Amendment IS enclosed. (Claims added by t h ~ s amendment have been properly numbered consecutively beginning with the number nextfollow~ng highest numbered original clalm in the prior appllcation.) the

12. [7 A new Disclosure Statement is enclosed. Applicant(s)' Disclosure Statement is as filed with the parent applicatlon (copy attached)

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081378,998 as originally filed on 1 hereby verify that the attached papers are a true copy of prlor application Serial No. ,wlth the exception that the attorney's docket number in the January 27,1995 lower left-hand corner of each paper has been adjusted t o reflect the instant application.
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The undersigned declares further that all statements made herein of h~slher own knowledge are true and that all statements made on information and belief are believed to be true; and furtherthat these statements were made wlth,the knowledge that willful false statements may jeopardize the validit"yf the application or any patent issuing thereon.

/0-/8- n / /rS (Date)

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FABRICATED ARTICLES MADE FROM ETHYLENE POLYMER BLENDS

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Cross-Reference to Related Ap~lica tions continuation-in-part of 5,272,1~& ,130, filed October i5 199l0and is A * U s $ fl27g.z7 z rial number 07/939,281 ent~tled , 4 . l y v r s " filed September 2 :1&2 no. u.s. F N 4 . : A 5, 278,272. W. Knight, John R. Wilson f each of which is reference. This application is 1number 08/010,958, filed . S. Kolthammer and Robert lymerizations, the by reference.
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Field of the ~nvention This invention relates to iompositions comprising speciIic ethylene/a-olefin polymer blends. / THe polymer blends preferably comprise: (A) at least one homogeneously branched substantially linear ethylene/ a-olefin in terpolymer having specific processing
(B) a heterogeneously branched ethylene polymer. Such compositions are particularly useful in film applications (e.g., high strength thin gauge packaging film or heat
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Background of the Invention Thin film products fabricated from linear low density polyethylene (LLDPE) and/or high density polyethylene (HDPE) are widely used for packaging applications such as merchandise bags, grocery sacks, and industrial liners. For these applications, films with high tensile strength, as well as high impact strength, are desired

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because film producers can down gauge their film products and still ' retain packaging performance. Previous attempts were made to optimize film tensile strength and yield strength by blending various heterogeneous 5 polymers together on theoretical basis. While such blends exhibited a synergistic response to increase the film yield strength, the film impact strength followed the rule of mixing, often resulting in a , "destructive synergism" (i.e., the film impact strength was actually lower than film made from one of the two components used to make 10 the blend). For example, it is known'that while improved modulus linear poly>thylene resin can be produced by blending high density polyethylene with a very low density polyethylene (mDPE), the impact strength of the resin blend follows the rule of mixing.

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There is a continuing need to develop polymers which can be formed into fabricated articles (e.g., film) having these - --combinations of properties (e.g., improved modulus, yield strength, impact strbgth and tear strength). The need is especially great for polymers which can be made into film which can also be down 20 gauged without loss of strength properties, resulting in savings for .film manufacturers and consumers, as well as protecting the environment by source reduction. Surprisingly, we have now discovered that film can have synergistically enhanced physical properties, when the film is 25 made from a blend of,at least one homogeneously branched ethylene/a-olefin interpolymer and a heterogeneously branched ethylene/a-olefin interpolymer.
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Brief Description of the Drawings Figure 1 shows the relationship between the density and the slope of strain hardening coefficient for homogeneously branched substantially linear ethylene/a-olefin interpolymers used in the compositions disclosed herein, in comparison with a heterogeneously branched ethylene/a-olefin copolymer.
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Figure 2 shows the short chain branching distribution a (as measured by analytical tempegulte rising elution fractionation (ATREF)) for a homogeneously branched substantially linear ethylehe/l-octene copolymer used in the invention, in comparison with DowlexTM 2045 (a heterogeneously branched ethylene/l-octene copolymer made by The Dow Chemical Company).
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Summary of the Invention , Formulated ethylene/ a-olefin compositions have now 10 been discovered to have improved physical and mechanical strength and are useful in making fabricated articles. Films made,from these '--. novel compositions exhibit surprisingly good impact and'tensilel properties, and an especially good combination of modulus ,yield, ultimate tensile, and toughness (e.g.pa t i pact). t 15 The compositions compris~from about 10 percent (by weight of the total composition) to about 95 percent (by weight _ the- -of total composition) of ( ' , m a t least one homogeneeusly'branched substantially linear ethylene/a-olefin in terpolymer having: 20 (i) a density from about 0.89 grams/cubic centimeter (g/cm3) to about 0.92 g/cm3, (ii) a molecular weight distribution (Mw/Mn) from about 1,8 to about 2.8, (iii) a melt index (12) from about 0.001 grams/lO 25 minutes (g/10 min) to about 10 g/10 min, (iv) no linear polymer fraction, and (v) a single melting peak as measured using differential scanning calorimetry; and (B) at least one heterogeneously branched ethylene 30 ' polymer having a density from about 0.93 g / m 3 to about 0.965 g/m3. In another aspect, the compositions comprise from about 10 percent (by weight of the total composition) to about 95 percent (by weight of the total composition) of :

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(A)'at least one homogeneously branched line

ethylene1a-olefin interpolymer having: (i) a density from about 0.89 grams/cubic cen (g/cm3).to about 0.92 g/cm3, 5 (ii) a molecular weight distribution ( M ~ / M from ~) about 1.8 to about 2.8, (iii) a melt index (12) from about 0.001 grams/\O minutes (g/10 min) to about 10 g/10 min, (iv) no linear polymer fraction, and \ (v) a single melting peak as measured using differential scanning calorimetry; and

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(B), at least one heterogeneously branched ethylene polymer having a density from about 0.93 g/an3 to about 0.965 g/cm3.
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Preferably, both the homogeneousli branched substantially linear ethylene/u-olefin interpolymer and the homogeneously branched linear ethylene/a-olefin interpolymer each have a slope of- - strain hardening coefficient greater than or equal to about 1.3.
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Detailed Descriotion of the Invention , ' 20' The homogeneously branched ethylene/a-olefin interpolymer is preferably a homogeneously branched substantially linear ethylene/a-olefin interpolymer as described in pewlmg USSN . S . f d r * t d@. 5.27~236 Bt3 07/776,13OA The homogeneously branched ethylene/a-olefin ,(,1197 interpolymer can also be a linear ethylene/a-olefin interpolymer as 25 described in USP 3,645,992 (Elston), the disclosure of which is incorporated herein by reference. The substantially linear ethylene/a-olefin interpolymers . are not "linear" polymers in the traditional sense of the term, as used to describe linear low density polyethylene (e.g., Ziegler polymerized 30 linear low density polyethylene (LLDPE)), nor are they highly branched polymers, as used to describe low density polyethylene (LDPE). The substantially linear ethylene/a-olefin interpolymers of the present inventionm d dherein defined as in copending application are . 5,272,23( ,no@ u,s rBt' serial number 07/776,130 and in copending application entitled "Elastic ,Ir7 197 I\
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Substantially Linear Olefin Polymers" filed September 2, 1992 in the names of Shih-Yaw Lai, George W. Knight, John R. Wilson and James C. Stevens. , The homogeneously branched ethylene/a-olefin interpolymers useful for forming the compositions described herein are those in which the comonomer is randomly distributed within a given interpolymer molecule and wherein substantially all of the , interpolymer molecules haye ene/comonomer ratio within that interpolymer. The of the interpolymers is 10 typically described by the SCBDI (Short Chain Branch Distribution , Index) or CDBI (Composition Distribution Branch Index) and is defined as the wkght percent of the polymer molecules having a c?monomer content within 50 percent of the median total molar comonomer content. The CDBI of a polymer is readily calculated from data obtained i 15 from techniques known in the art, such as, for example, temperature rising elution fractionation (abbreviated herein as "TREF'I) as described, for example, in Wild et a1 Journal of Polymer Science, Polv. Phys. Ed., ~ o l ? 2 0p. 441 (1982), in U.S. Patent 4,798,081 (Hazlitt et al.), or in U.S. , Patent 5,089,321 (Chum et al.) the disclosures of all of which are 20 incorporated herein by reference. The SCBDI or CDBI for the linear and for the substantially linear olefin polymers of the present invention is preferably greater than about 30 percent, especially greater than about 50 percent. The homogeneous ethylene/a-olefin polymers used in this invention essentially lack a measurable "high density" fraction as 25 measured by the,TREF technique (i.e., the homogeneously branched ethylene/a-olefin polymers do not contain a polymer fraction with a degree of branching less than or equal to 2 methyls/1000 carbons). the^ homogenebusl{ branched ethylene/a-olefin polymers also do not contain any highly short chain branched fraction (i.e., the 30 homogeneously branched ethylene/a-olefin polymers do not contain a ~olymer fraction with a degree of branching equal to or more than about 30 methyls/1000 carbons). The substantially linear ethylene/a-olefin interpolymers for use in the present invention typically are interpolymers of ethylene

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with at least one C3-C20 a-olefin and/or Cq-C1g diolefins. Copolymers of ethylene< I-octene are especially preferred. The term and "interpolymer" is used herein to indicate a copolymer, or a terpolymer, or the like. That is, at least one other comonomer is polymerized with , ethylene to make the interpolymer. Ethylene copolymerized with two or more comonomers can also be used to make. the homogeneously branched substantially linear interpolymers useful in this invention. Preferred comonomers include the C3-C20 a-olefins, especially propene,
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isobutylene, 1-butene, 1-hexen$, 4-methyl-1-pentene, 1-heptene, 110 octene, 1-nonene, and 1-decene, more preferably 1-butene, 11-hexene, 4methyl-1-pentene and 1-octene. , . -\The term "linear ethylene/a-olefin interpolymer" means that the interporymer does not have long chain branching. That is, the linear- ethylene/a-olefin interpolymer has an absence of long chain . 15 branching, as for example the linear low density polyethylene polymers or linear high density polyethylene polymers made using unifonm (i.e., homogeneous) branching distribution polymerization processes (e.g., as e described in USP 3,645,992 (Elston)) and are t h ~ s in which the comonomer is randomly distributed within a given interpolymer 20 molecule and wherein substantially all of the interpolymer molecules have the same ethylene/comonomer ratio within that interpolymer. The term "linear ethylene/a-olefin interpolymer" does not refer to high pressure branched (free-radical polymerized) polyethylene which is known- to those skilled in the art to have numerous long chain 25 branches. The branching distribution of the homogeneously branched linear ethylenela-olefin interpolymers is the same or substantially the same as that described for the homogeneously branched substantially linear ethylene/a-olefin interpolymers, with the exception that the linear ethylene/a-olefin interpolymers do not have any long chain 30 branching. The homogeneously branched linear ethylene/a-olefin interpolymers comprise ethylene with at least one C3-C20 a-olefin and/or C4-Cl8 diolefin. Copolymers of ethylene and 1-octene are especially preferred. Preferred comonomers include the C3-C20aolefins, especially propene, isobutylene, 1-butene, 1-hexene, 4-methyl-l0
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. pentene, 1-heptene, 1-octene, 1-nonene, and 1-decene, more prefe
1-butene, 1-hexene, 4-methyl-1-pentene and 1-octene. Both the homogeneously branched substantially line and linear ethylene/a-olefin interpolymers have a single melting point, as opposed to traditional heterogeneously branched'ziegler polymerized ethylene/a-olefin copolymers having two or more melting points, as determined using differential scanning calorimetry (DSC). I The density of the homogeneously branched linear or substantially linear ethylene/a-olefin interpolymers (as measured in accordance with ASTM D-792) for use in the present invention is generally from about 0.89 g/an3 to about 0.935 g/cm3, preferably from about 0.905 g/cm3 to about 0.925 g/cm3, and espe$ally from about 0.905 g/an3 to less than about 0.92 g/cm3. The amount of the homogeneously branched linear or substantially linear ethylene/a-olefin polymer incorporated into the -. compositioh varies depending upon the heterogeneously branched ethyleqp polymer to which it is combined. Howevey, about 50 percent (by weight of the total composition) of the homogeneous linear or' substantially linear ethylene/a-olefin polymer is especially preferred in the novel compositions disclosed herein. The molecular weight of the homogeneously branched linear or substantially linear ethylenela-olefin interpolymers for use in the present invention is conveniently indicated using a melt index measurement according to ASTM D-1238, Condition 190*C/2.16 kg (formerly known as "Condition (E)" and also known as 12). Melt index is inversely proportional to the molecular weight of the polymer. Thus, the higher the molecular weight, the lower the melt index, although the relationship is not linear. The lower melt index limit for the homogeneously branched linear or substantially linear ethylene/aolefin interpolymers useful herein is generally about 0.001 grams/lO minutes (g/10 min). The upper melt index limit for the homogeheously branched linear or substantially linear ethylene/a-olefin interpolymers
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is about loJg/lO min, preferably less than about 1 g/10 min, and especially less than about 0.5 g/10 min. Another measurement useful in characterizing the 'ly molecular weight of the homogeneously branched linear ar 5 linear ethylene/a-olefin interpolymers is conveniently indicated using a - . melt index measurement according to ASTM D-1238, Condition 190eC/10kg (formerly known as "Condition (N)" and also known a s 110). The ratio of the 110 and I2 melt index terms is the melt flow ratio and is designatid as I10/12. Generally, the Ilo/I2 ratio for the 10 homogeneously branched linear ethylene/a-olefin interpolymers is about 5.6. For the homogeneously branched substantially linear ethylene/cc-olefin interpolymers used in the compositions of the invention, the 110/12 ratio indicates the degree of long chain branching, i.e., the higher the I101/12 ratio, the more long chain branching in the 15 interpolymer. Generally, the I10/12 ratio of the homogeneously ; brandyd substantially linear ethylene/a-olefin interpolymers is at least about 6d preferably at least about 7, especially at least about 8 or above. For the homogeneously branched substantially linear ethylene/a-olefin interpolymers, the higher -the Ilo/I2 ratio, the better the processability. 20 Other additives such as antioxidants (e.g., hindered phenolics (e.g., lrganox@1010 made by Ciba Geigy Corp.), phosphites (e.g., lrgafos@168 also made by Ciba Geigy Corp.)), ding additives (e.g., PIB), antiblock additives, pigments, fillers, and the like can also be included in the formulations, to the extent that they do not interfere 25 with the enhanced formulation properties discovered by Applicants.
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Molecular Weight Distribution Determination The molecular weight distribution of the linear or substantially linear olefin interpolymer product samples is analyzed by gel permeation chromatography (GPC) on a Waters 150C high temperature chromatographic unit equipped with three mixed porosity columns (Polymer Laboratories l03,104,l05, and 106), operating at a system temperature of 140°C. The solvent is 1,2,4-trichlorobenzene, from which 0.3 percent by weight solutions of the samples are prepared

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for injection. The flow rate is 1.0 rnilliliter/minute and the injection size is 200 microliters. A differential refractometer is being used as the detector. The molecular weight determination is deduced by using narrow molecular weight distribution polystyrene standards (from Polymer Laboratories) in conjunction with their elution volumes. The equivalent polyethylene molecular weights are determined by using appropriate Mark-Houwink coefficients for polyethylene and polystyrene (as described by Williams and Word in Journal of Polymer Science, Polymer Letters, Vol. 6, (621) 1968, incorporated herein by reference) to derive the following equation:
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Mpolyethylene = a '( ~ ~ o l ~ s t ~ r e n e ) ~ .

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In this equation, a ='0.4316 and b = 1.0. Weight average molecular weight, Mw, is calculated the usual manner according to the . following formula: Mw = R wi' Mi, where wi and Mi are the weight , fraction and molecular weight, respectively, of the ith fraction eluting from the GPC column. For both the homogeneously branched linear and substantially linear ethylene/a-olefin polymers, the molecular weight distribution (Mw/Mn) is preferably from about 1.8 to about 2.8, more preferably from about 1.89 to about 2.2 and especially about 2.

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tion of the Slove of Strain Hardening Coefficient The slope of strain hardening is measured by compression molding a plaque from the polymer to be tested. Typically, the plaque is molded at about 177OC for 4 minutes under almost no pressure and then pressed for 3 minutes under a pressure of about 200 psi. The plaque is then allowed to cool at about 8OC/minute while still under 200 psi pressure. The molded plaque has a thickness of about 0.005 inches. The plaque is then cut into a dogbone shaped test piece using a steel rule die. The test piece is 0.315 inches wide and 1.063 inches long. The start of the curved portion of the dogbone shape begins at 0.315 inches from each
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end of the sample and gently curves (i.e., tapers) to a width of 0.09 inches. The curve ends at a point 0.118 inches from the start of the curve such that the interior portion of the dogbone test piece has a width of 0.09 inches and a length of 0.197 inches. The tensile properties of the test sample is tested on an Instron Tensile Tester at a crosshead speed of 1 inch/minute. The slope of strain hardening is calculated from the resulting tensile curve by drawing a line parallel to the strain hardening region of the resulting stress/strain &rve. The strain hardening region occurs after the sample has pdled it? initial load ((i.e., stress) usually with little or no elongation , during &e$itial load) and after the sample has gone through a slight drawing stage (usually with little or no increase in load, but with increasing elongation (i.e., strain)). In the strain hardening region, the load and the elongation of the sample both continue to increase. The load increase? in the strain hardening region at a much lower rate than during the &$a1 load region and the elongation also increase, again at-a rate lower than that experienced in the drawing region. Figure 1 shows 4 the various stages of the stress/strain curve used to calculate the slope of strain hardening. The slope of the parallel line in the strain hardening region is then determined. The slope of strain hardening coefficient (SHC) is calculated according to the following equation: SHC = (slope of strain hardening) * (12)0-25 where I2 = melt index in grams/lO minutes. For both the homogeneously branched linear and substantially linear ethylene/a-olefin interpolymers used in the invention; the SHC is greater than about 1.3, preferably greater than about 1.5. Surprisingly, the slope of strain hardening coefficient reaches a maximum for the linear or the substantially linear ethylene/aolefin polymers at a density from about 0.89 g/cm3 to about 0.935 g/an3. Heterogeneous ethylene/a-olefin polymers, in contrast, do not behave in the same manner. Figure 1 graphically depicts the relationship between the density of the homogeneously branched substantially linear
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The ~ e t e r h ~ e n e o u sBranched Ethylene Polymer ly The ethylene polymer to be combined with the homogeneous ethylene/a-olefin interpolymer is a heterogeneou 5 branched (e-g., Ziegler polymerized) interpolymer of ethylhe w least one C3-C20 a-olefin (e.g., linear low density polyethylene (LLDPE)). Heterogeneously branched ethylene/a-olefin J interpolymers differ from the homogeneously branched ethylene/aolefin interpolymers primarily in their branching distribution. For 0 example, heterogeneously branched LLDPE polymers have a distribution of branching, including a highly branched portion (similar to a very 1o;'de~sity polyethylene), a medium branched portion (similar to a medium branched polyethylene) and an essentially linear portion (similar to linear homopolymer polyethylene). The amount of 15 each of these fractiond varies depending upon the whole polymer proper ties desired. For example, linear homopolymer polyethylene has neither branched nor' highly branched fractions, but is linear. A v e j ;ow deilsity heterogeneous polyethylene having a density from about 0.9 g/an3 to about 0.915 g/cm3 (such as ~ t t a n e @ copolymers, sold by 20 The Dow Chemical Company and ~lexomer@ by Union Carbide sold Corporation) has a higher percentage of the highly short chain branched fraction, thus lowering the density of the whole polymer. Heterogeneously branched LLDPE (such as owle ex@ sold by The Dow Chemical Company) has a lower amount of the highly1 25 branched fraction, but,has a greater amount of the medium branched fraction. Figure 2 graphically depicts the relative amounts of these various fractions (as measured using temperature rising elution fractionation) for owl ex@ 2045 (a heterogeneously branched ethylene/l-octene copolymer having a melt index (12) of about 1 g/10 30 min, a density of about 0.92 g/cm3, a melt flow ratio (I10/12) of about 7'93 and a molecular weight distribution (Mw/Mn) of about 3.34), as compared with a homogeneously branched substantially linear ethylene/l-octene copolymer having a melt index (12) of about 1 g/10 min, a density of about 0.92 g/cm3, a melt flow ratio (Ilo/I2) of about 10.5
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and a molecular weight distribution (Mw/Mn) of about 2.18. Note tha the homogeneously branched polymer has a single relatively narrow peak at an elution temperature of about 85OC, while the ~ o w l e x a 2045 polymerhas a br ad branching distribution, as represented by the -?*mpenatuR.e5 breadth of elution over which the polymer fractions elute. ~ o w l e x a 2045 also has a distinct peak at an elution temperature of about 98OC, indicating the "linear" fraction of the whole polymer. er which has the beneficial Increasing the fraction of the Can-\ ,m4 d increasing other fractions has not properties, without

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been demonstrated here-to-fore. Preferably, however, the heterogeneously branched ethylene polymer is a heterogeneously branched Ziegler polymerized ethylene/a-olefin interpolymer having no more than about 10 pe'rcent (by weight of the polymer) of a polymer fraction having a SHC 2 1.3. More preferably, the heterogeneously branched ethylene
,

15

polymer is a copolymer of ethylene with a C3-C20 a-olefin, wherein the (i) a density from about 0.93 g / m 3 to about 0.965 (ii) a melt index (12) from about 0.1 g/10 min to about 500 g/10 min, and (iii) no more than about 10 percent (by weight of the polymer) of a polymer fraction having a SHC 2 1.3. The(heterogeneously branched ethylene/a-olefin interpolymers and/or copolymers also have at least two melting peaks as determined using Differential Scanning Calorimetry (DSC). The Formulated Compositions The compositions disclosed herein can be formed by any convenient method, including dry blending the individual components and subsequently melt mixing or by pre-melt mixing in a separate extruder (e.g., a Banbury mixer, a Haake mixer, a Brabender internal mixer, or a twin screw extruder).

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Another technique for making the compositions in-sit n r d rbe*Jo disclosed in pending USSN 08/010,958, enti led Ethylene 4 Interpolymerizations, which was filed January 29,1993 in the n Brian W.S. Kolthammer and Robert S. Cardwell, the disclosure of which is incorporated herein in its entirety by reference. USSN,08/010,958, h a w describes, inter alia, interpolymerizations of ethylene and C3-C20 alphaolefins using a homogeneous catalyst in at least one reactor and a heterogeneous catalyst in at least one other reactor. The reactorsJcanbe operated sequentially or in parallel.

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t h e compositions can also be made by fractionating a heterogeneous ethylenela-olefin polymer into specific polymer fractions w,ith each fraction having a narrow composition (i.e., branching) distribution, selecting the fraction having the specified properties (e.g.; SHC 2 1.3), and blending the selected fraction in the appropriate amounts with another ethylene polymer. This method is obviously not as econ mica1 as the in-situ interpolymerizations of . a d USSN 08/010,958, but can be used to obtain the compositions of the invention.
&L46W.$

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Fabricated Articles Made from the Novel Comoositions Many useful fabricated articles benefit from the novel compositions disclosed herein. For example, molding operations can be used to form useful fabricated articles or parts from the compositions disclosed herein, including various injection molding processes (e.g., that described in Modern Plastics Encyclopedia/89, Mid October 1988 Issue, Volume 65, Number 11, pp. 264-268, '?ntroduction to Injection Molding" by H. Randall Parker and on pp. 270-271, "Injection Molding . Thermoplastics" by Michael W. Green, the disclosures of which are incorporated herein by reference) and blow molding processes (e.g., that described in Modern Plastics Encvclopedia/89, Mid October 1988 Issue, Volume 65, Number 11, pp. 217-218, "Extrusion-Blow Molding" by Christopher Irwin, the disclosure of which is incorporated herein by reference), profile extrusion, calandering, pultrusion (e.g., pipes) and the like. Rotomolded articles can also benefit from the novel compositions

EX. B PAGE 22

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5

2

10

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described herein. Rotomolding techniques are well known to those skilled in the art and include, for example, those described in Modern Plastics Encvclopedia/89, Mid October 1988 Issue, Volume 65, Number 1 , pp. 296-301, "Rotational Molding" by R.L. Fair, the disclosure of 1 which is incorporated herein by reference). Fibers (e.g., staple fibers, melt blown fibers or spunbonded fibers (using, e.g., systems as disclosed in USP 4,340363, USP 4,663,220, USP 4,668,566, or USP 4,322,027, all of which are incorporated herein by reference), and,gel spun fibers (e.g., the system disclosed in USP 4,413,110, incorporated herein by reference)), both woven and nonwoven fabrics (e.g., spunlaced fabrics disclosed in USP 3,485,706, incorporateti herein by reference) or structures made from such fibers (including, e.g., blends of these fibers with other fibers, e.g., PET or cotton)) can also be made from the novel compositions disclosed herein. Film and film structures particularly benefit from the novel compositions described herein and can be made using conventional hot blown film fabrication techniques or other biaxial -orientation processes such as tenter frames or double bubble processes. Conventional hot blown film processes are described, for example, in The Encvclopedia of Chemical Technolow Kirk-Othmer, Third Edition, John Wiley & Sons, New York, 1981, Vol. 16, pp. 416-417 and Vol. 18, pp. 191-192, the disclosures of which are incorporated herein by referepce. Biaxial orientation film manufacturing process such as described in a "double bubb1e"process as in U.S. Patent 3,456,044 (Pahlke), and the processes described in U.S. Patent 4352,849 (Mueller), U.S. Patent 4,597,920 (Golike), U.S. Patent 4,820,557 (Warren), U.S. Patent 4,837,084 (Warren), U.S. Patent 4,865,902 (Golike et al.), U.S. Patent 4,927,708 (Herran et al.), U.S. Patent 4,952,451 (Mueller), U.S. Patent 4,963,419 (Lustig et al.), and U.S. Patent 5,059,481 (Lustig et al.), the disclosures of each of which are incorporated herein by reference, can also be used to make film structures from the novel compositions described herein. The film structures can also be made as described in a tenter-frame
\

EX. B PAGE 23

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5

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10

15

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Other multi-layer film manufacturing techniques for food packaging applications are described in Packaping Foods With Plastics, by Wilmer A. Jenkins and James P. Harrington (1991), pp. 19-27, and in "Coextrusi'on Basics" by Thomas I. Butler, Film Extrusion Manual: Process, Materials, Properties pp. 31-80 (published by TAPPI Press (1992)) the disclosures of which are incorporated herein by reference. The films may be monolayer or multilayer films, The2 film made from the novel compositions can also be coextruded with the other layer($ or:the film can be laminated onto another layer(s) in a secondary operation, such as that described in Packaging: Foods With Plastics, b)r Wilmer A. Jenkins and James P. Harrington (1991) or that ' , described in "Coextrusion For Barrier Packaging" by W.J. Schrenk and C.R. Finch, Societv of Plastics Engineers RETEC Proceedin~s, June 15-17 (1981), pp. 211-229, the disclosure of which is incorporated herein by reference. If a monolayer film is produced via tubular film (i.e., blown film techniques) or flat-die(i.e., cast film) as described by K.R. Osborn and W.A. Jenkins in "Plastic Films, Technology and Packaging , Applications" (Technomic Publishing Co., Inc. (1992)), the disclosure of ' which is incorporated herein by reference, then the film must go through an additional post-extrusion step of adhesive or extrusion lamination to other packaging material layers to form a multilayer structure. If the film is a coextrusion of two or more layers (also 5 dyribed by Osborn and Jenkins), the film may still be laminated to additional layers of packaging materials, depending on the other physical requirements of the final film. "Laminations Vs. Coextrusion" by D. Dumbleton (conv6rting Magazine (September 1992), the 5 disclosure of which is incorporated herein by reference, also dj\cusses ' lamination versus coextrusion. Monolayer and coextruded films can also go through other post extrusion techniques, such as a biaxial orientation Drocess. Extrusion coating is yet another technique for producing multilayer film structures using the novel compositions described herein. The novel compositions comprisetat least one layer of the film structure. Similar to cast film, extrusion coating is a flat die technique.
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EX. B PAGE 24

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-18-

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5

10
,

A sealant can be extrusion coated onto a substrate either in the form of a monolayer or a coextruded extrudate. Generally for a multilayer film structure, the novel , compositions described herein comprise at least one layer of the total multilayer film structure. Other layers of the multilayer structure include but are not limited to barrier layers, and/or tie layers, and/or structural layers. Various materials can be used for these layers, d t h some of them being used as mdre than one layer in the same film structure. some of these materials include: foil, nylon, ethylene/vinyl alcohol, (EVOH) copolymers, polyvinylidene chloride (PVDC), polyethylenterep alate (PET), oriented polypropylene (OPP), "h ethylene/vinyl ateta te (EVA) copolymers, ethylene/acrylic acid (EAA) copolymers, ethylene/methaaylic acid (EMAA) copolymers, LLDPE, HDPE, LDPE, nylon, graft adhesive polymers (e.g., maleic anhydride grafted polyethylene), and paper. Generally, the multilayer film structures comprise from 2 to about 7 layers.
i

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~xam~li 1 20 Seventy five percent (by weight of the total composition) of a homogeneously branched substan tially linear ethylene/ 1-octene copolymer having 12 of about 1 g/10 min, density of about 0.91 g/an3, I10/12 of about 10, Mw/Mn of about 2, and SHC of about 1.81 is dry ,
_- Mended and then melt blended with 25 percent (by weight of the total

. 25

30

composition) of a heterogeneously branched ethylene/ 1-octene copolymer having I2 of about 1g/10 min, density of about 0.935 g/an3, 110/12 of about 7.8, and Mw/Mn of about 3.4. The heterogeneously branched ethylene/l-octene copolymer has a fraction of about 5 percent (by weight of the haterogeneously branched copolymer) having a SHC 2 1.3. The dry blend is tumble blended in a 50 gallon drum for about 1 hour. The melt blend is produced in a ZSK 30 twin screw extruder (30 mm screw diameter) and is then fabricated into film. The final blended composition has a density of about 0.919 g/cm3.

C-40,121-B G ~ L

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':

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The blended composition is then fabricated into blown having a thickness of about 1 mil on an Egan Blown Film Line havin 2 inch diameter screw, a 3 inch die and at a 2.5 inch blow up ratio (BUR) as described in Table 2. For all film samples in Examples 1,2,4, and 6 and for comparative examples 3,5, and 7, the targeted gauge is about 1 mil, using a blow-up ratio (BUR) of 2.5:1, a LLDPE screw design is used, a die gap of 70 mils is used, and a lay flat of about 11.875 inches is used. J Film properties are measured and reported in Table 3 with other examples of the invention and with comparative examples. Dart impact (type A) of the films is measured in accordance with ASTM D1709-85; tensile strength, yield, toughness, and 2% secant modulus of the films is mebured in accordance with ASTM D-882; Elmendorf tear (type B) is measured h accordance with ASTM D-1922; PFT tear is measured in accordance with ASTM D-2582; Block is measured in accordance with ASTM D-3354. Puncture is measured by using an Instron tensiometer Tensile Tester with .an integrator, a specimen holdkr that holds the film sample,taut.across a circular opening, and a rod-like puncturing device with a rounded tip (ball) which is attached to the cross-head of the ' Instron and impinges perpendicularly onto the film sample. The Instron is set to obtain a crosshead speed of 10 inches/minute and a chart speed (if used) of 10 inches/minute. Load range of 50% of the load cell capacity (100 lb. load for these tests) should be used. The puncturing device is installed to the Instron such that the clamping unit is attached to the lower mount and the ball is attached to the upper mount on the crosshead. Six film speamens are used (each 6 inches square). The specimen is clamped in the film holder and the film holder is secured to the mounting bracket. The crosshead travel is set and continues until the specimen breaks. Puncture resistance is defined as the energy to puncture divided by the volume of the film under test. Puncture resistance (PR) is calculated as follows: 'PR = E/((12)(T)(A)) where PR = puncture resistance (ft-lbs/in3)
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-19-

EX. B PAGE 26

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I
E
= energy

(inch-lbs) = area under the load displacement

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curve
12 = inches/foot
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T = film thickness (inches), and A = area of the film sample in

2.56 in2.

Example 2

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Seventy five percent (by weight of the total composition) of a homogeneously branched substantially linear ethylene/l-octene copolymer having I2 of about 0.5 g/10 min, density of about 0.915 g/an3, I10/12 of about 11, Mw/Mn of about 2.4, and SHC of about 2.265 is dry blended andXthen,melt blended (as described in Example 1)with 25 percent (by weight of .the total composition) of a heterogeneously branched ethylene/l-octene copolymer having I2 of about 1 g/10 min, density of about 0.935 g/cm3, I10/12 of about 7.8, and Mw/Mn of about 3.4. The heterogeneously branched ethylene/l-octene copolymer has a fraction of about 5 percent (by weight of the heterogeneously branched copolymer) having a SHC 2 1.3. The final blended composition has a density of about 0.92 g/cm3. Blown film is made as described in Table 2 and film properties are measured and reported in Table 3 with other examples of the invention and with comparative examples. comparative Example 3 A heterogeneously branched ethylene/l-octene copolymer having I2 of about 1 g/10 min, density of about 0.92 g/cm3, I10/12 of about 7.93, and Mw/Mn of about 3.34 is made into film as described in Example 1. The heterogeneously branched ethylene/l-octene copolymer has a fraction of about 36 percent (by weight of the heterogeneous copolymer) having a SHC 2 1.3. The entire heterogeneous ethylene/loctene copolymer has a SHC of about 1.5. Blown film is made as described in Table 2 and film properties are measured and reported in Table 3 with other examples of the invention and with comparative examples.
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Example k
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E ample 4 is an in-situ blend made according to

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08/010,958, wherein the homogeneously branched substantial I\ polymer is made in a first reactor and is an ethylene/l-octhe having a melt index (12) of about 0.5 g/10 min., and a density 0.9054 g/cm3, a melt flow ratio (110/12) of about 8.27 and a molecular weight distribution (Mw/Mn) of about 1.979 and comprises about 50% (by weight of t+e total compos&ion). A heterogeneously branched ethylene/l-octene copolymer is made in a second reactor operated sequentiauy with the first reactor and has a melt index (12) of about 1.5 g/10 min., ahd a density of about 0.944 g/an3 and comprises the remaining 50% (by weight of the total composition). The total composition has a melt index (12) of about 1 g/10 min., a density of about 0.9248 g/cm3, a melt flow ratio (110/12) of about 7.22 and a molecular weight distribution (Mw/Mn) of about 2.641. This composition is made into blown film as described in Table 2 and the resultant film properties are reported in Table 3. Comparative Example 5 Comparative Example 5 is an ethylene/)-octene copolymer /l*r & M q c . 3 SO,^,^ made according to USSN 07/773,375, filed October 7,1991,h the disclosure of which is incorporated herein by reference. About 15% (by weight of the total composition) is made in a first reactor, I.with the remaining portion of the composition polymerized in a second sequentially operated reactor. ~ 0 t reactors utilize Ziegler type catalysts and make h heterogeneously branched polymers. The total composition has a melt index (12) of about 0.56 g/10 min., a density of about 0.9256 g/cm3, a melt flow ratio (I10/12) of about 9.5 and a molecular weight distribution (Mw/Mn) of about 4.35. This composition is also made into blown film as described in Table 2 and the resultant film properties are reported in Table 3.
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EX. B PAGE 28

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Examvle 6

6

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Ex m le 6 is an in-situ blend made according to USSN 08/010,958, wherein the homogeneously branched substantially linear n b polymer i s made in a first reactor and is an ethylene/l-octqne co~lymer having a fractional melt index (12) ,a density of about 0.906 g/an3, a melt flow ratio (Ilo/12) of about 8-10 and a molecular weight distribution (Mw/Mn) of about 2.2 and comprises about 43% (by weight of the total composition). A second heterogeneously branched ethylene/l-octene ifzea~tcopolymer is made in a second ieestst operated sequentially with the first reactor and has a melt index (12) of about 0.85 g/10 minutes, a
now

r b h h ~ dP

15

density of about 0.938 g / m 3 and comprises the remaining 57% (by '. . weight of the total composition). The total composition has a melt index &).of about 0.53 g/10 minutes, a density of about 0.9246 g/an3, a melt flow ratio (110/12) of about 7.83, and a molecular weight distribution (Mw/Mn) of about 2.8. This composition is made into blown film as described in Table 2 and the film properties are reported in Table 3. Comparative Example 7 Comparative Example 7 is an ethylene/l-octene copolymer h m uu.s P C t s ~ t d 5 a . 5 0 ~ 6 1 ~ . made according to USSN 07/773,375, filed October 7,1991,4 the discfosure of which is incorporated herein by reference. About 25% (by weight of the total composition) is made in a first reactor, with the remaining portion of-the composition polymerized in a second sequentially operated reactor. Both reactors utilize Ziegler type catalysts and make heterogeneously branched polymers. The total composition has a melt index (12) of about 0.49 g/10 min., a density of about 0.9244 g/m3, a melt flow ratio (110/12) of about 10 and a molecular weight distribution (Mw/Mn) of about 4.78. This composition is also made into blown film as described in Table 2 and the resultant film properties are reported in Table 3.

7

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EX. B PAGE 29

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5

Comparative Examwle 8 , Comparative example 8 is a heterogeneously branched ethylene/l-octene copolymer having a melt index (12) of about 1 g/10 bo u f minutes, a density of 0.9249 g / ~ 3 a, melt flow ratio (110/12) of about 8 aGd a molecular weight distribution (Mw/Mn) of about 3.5. Blown film is made as described in Table 2 and film properties are measured and reported in Table 3 with other examples of J the invention and comparative examples.
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EX. B PAGE 30

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*NR = Not recorded

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5

In general, films made from the novel formulated ethylene/ a-olefin compositions exhibit good impact and tensile properties, and an especially good combination of tensile, yield and toughness (e.g., toughness and dart impact). Further, films from the example resins exhibited significant improvements over films made from the comparative resins in a number of key propertib.

I

:

For example, comparing examples 1 and 2 with comparative example 3, the data show films produced from the melt , 10 blends (examples 1 and 2) exhibited significantly higher values for the m following film properties: dart pact, MD tensile, CD tensile, MD 6-D toughness, CD toughness MD ppt tear, Be ppt tear, CD Elmendorf tear B, punctureand significantly lower block. Comparing example 4 to comparative example 5,?the data 115 show films roduced from the in-situ blend (made according to USSN .Pcld.4 08/010,958) exhibited significantly higher values for the following film 4 properties: dart impact, MD toughness and CD toughness. ... Comparing example 6 to comparative examples 7 (an haw u.5. ~~ 5,25b,6t~ ethylene/l-octene copolymer made according to USSN 07/773,375) and d 20 8 (an heterogeneously branched ethylene/l-octene copolymer), the data show films produced from the in-situ blend (made according to USSN ,08/010,958) exhibited significantly higher values for the following film properties: dart impact, MD yield, CD yield, MD tensile, CD tensile, CD Elmendorf tear B and puncture and significantly lower block.
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We Claim: ymer composition, percent (by weight o the totaf composition) to about 95 percent composition) of :

J

s/cubic centimete -. (g/cm3) to about 0.92 g/cm3, n (Mw/Mn) from

10

about 1.8 to about 2.8, ' .

2. The film claim 1 wherein the homogeneously branched substantially inear ethylene/a-olefin interpolymer has a slope of strain hard ing coefficient greater than or equal to about 1.3.

The film of claim 1 wherein the heterogeneously branched ethylene polymer is an interpolymer of ethylene with at least one C3-C20 a-olefin. The film of claim 1 wherein the homogeneously branched substantially linear ethylenela-olefin interpolymer is an interpolymer of ethylene with at least one C3-C20 a-olefin.
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I

claim 1 wherein the homogeneously branched.substantially linear ethylene/a-olefin interpolymer is a copolymer of ethylene and a C3-C20 a-olefin.
b The film of claim $wherein the homogen,eously branched substantially linear ethylene/a-olefin copolymer is a copolymer of ethylene and 1-octene.
\

b ~ The film of :

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34 - The film of claim ,&wherein the heterogeneously
10 branched ethylene polymer is a copolymer of ethylene and a C3C20 a\*

3-

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The film of claim 8 wherein the heterogeneously ' branched-ethylene polymer is a copolymer of ethylene and 1-octene. e polymer composition,

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1

(g/cm3) to about 0.92 g/cm3,

bution (Mw/Mn) from
25

about 1.8 to about 2.8, about 0.001 grams/lO

a single melting peak as measured using about 5 percent (by weight of the total

C-40,12143& L

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least one homogeneously -olefin interpolymer having: about 0.89 grams/cubic centimeter (g/cm3) to about 0.92 g/cm3, about 1.8 to about 2.8, om about 0.001 grams/lO
l
-

t distribution (M&/Mn) from

a single melting peak as measured using

m 17 wherein the ear ethylene/a-olefin g coefficient greater than or 0
( ,I

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The improvement of claim Wwherein the homogeneously branched substanti~lly linear ethylene/a-olefin interpolymer is an interpolymer of ethylene with at least one C3olefin.

4

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1 O28. The improvement of claim A 7 wherein the homogeneously branched substantially linear ethylene/a-olefin interpolymer is a copolymer of ethylene and a C3-Czo a-olefin.
1

2 The improvement of claim .

*wherein the
B

homogeneously branched substantially linear ethylene/a-olefin interpolymer is a copolymer of ethylene and 1-octene.
30
/

The improvement of claim # wherein the heterogeneously branched ethylene polymer is a copolymer of ethylene and a C3-C20 a-olefin.

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1 3 2 The improvement of claim Z? % wherein the
heterogeneously branched ethylene polymer is a copolymer ofrethylene
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(g/cm3) to about 0.92 g/cm3, (ii) a molecular w about 1.8 to about 2.8,
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EX. B PAGE 38

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Case 1:05-cv-00737-JJF
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Document 162-3
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T ~ I Dedaratlon and Power of Attorney l S

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DECLARATIOI - AND POWER OF ATTORNEY
AS a below

3 ii ; ; {
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USAIPCT

(a) (b) Iverily believe I amlwe are the original, first and soleljoint inventor(s) of the subject matter which is embrked by and for which a patent is sougilt on the invention entitled: and the speo;fication of which: (check one)
'

named inventor, I hereby declare that: My residence and Citizenship are as stated below my name. My P.O. (mading) address is the same as my residence unless otherwise stated.

FABRICATED ARTICLES MADE FROM ETHYLENE POLYMER BLENDS
is attached hereto (C- ).
was filed on April Application No

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28, 1993 08/054379

as (c- 40,121-G).

and was amended on

I hereby state that I have reviewed and understand the contentsof the above identified specification, including the cl amendment referred to above. ) Iacknowledge my duty under 37 C R 1.56 to disclose to the U.S. Patent and Trademark Office all infor F patentability as defined in 37 C R 1.56(b). Iacknowledge the same duty of disclosurewith respect to F which arises after the filing date of any prior application claimed under paragraph (f) t o the extent t h application i s not disclosed i n the prior United States application. (e) Ihereby claim foreign priority benefits under Title 35, United States Code 5 119 of any foreign application(s) for patent or inventor's listed below and have also identified below any foreign application for patent or inventor's certificate having a filing date before t h application on which priority is claimed? PRIORITY CLAIMED PRIOR FOREIGN APPLICATION(S)
Number (f) \Country DayIMonttllYear t ~ l e d

- ' s Y ' Em

I hereby Cla~m beneflt under the

07/776,130
Appllcatlon 5erlal No

he 35, Un~ted Code 5 120 of any Un~ted appl~cat~ons(s) below: States States llsted
October 15,1991
hllng Vate

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Pending

>tatus (Patented, Pendlng, Abandoned)

I hereby appo~nt following attorney(s) andlor agent(s) to prosecutet h ~ s the appl~cat~on to transact ail busmess In the Patent and Trademark and Off~ce connected therew~th. Address all correspondence to: THE DOW CHEMICAL COMPANY. Patent Dept,, 8-1211 Freeport, TX 77541 and telephonic , communlcatlonst o the followlnq:
(1)

Stephen P. Krupp

/

3-

7

(TEL (409)238-2889
-

Reg Reg Reg Reg

No 34,366 No, xb,413 No 27,204 No. 20,128

This appointment, including the rlght t o delegate this appo~ntment, shall also apply t o the same extent t o any proceedings established by the Patent Cooperatiorl Treaty. that all statements made herein of my own knowledge are true and that all starements made on ~nforrnat~on belref are bel~eved and further that these statements were made with the knowledge that willful false statements and the Itkeso made are pun~shable flne OF by or both under Tttle 18, United States Code 5 1001 and that such w ~ l l f ufalse statements may jeopard~ze val~dlty the appllcatlon or l the of Inventor(s):

9

nt Freeport, Texas 17541; U.S.A
this

7 ' 4

day of

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Freeport, Texas 77541, U.S.A.

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9

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t h ~ s f ? f L dayof S~gnature

S~gnature

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I m e : Residence: ~ l t yState, ZIP: . Country: C~t~zenship: P.O. Address:

FUII Name:

-Ronald_P. Markovich

x-0
7y

126 Juniper Street Lake Jackson,Texas 77566 - j ' j ~ United States of America United States of America Same as Residence

Res~dence: 1403 Bayou Oak Drive clty, State, zipLFriendswood. Texas 77546 Country: United States of America C~t~zensh~p: United States of America P.O. Address: Same as Residence

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Freeport, Texas 77541, U.S.A.

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Texas 77541, U.S.A.
day of

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Residence: City, State, ZIP:. Country:

Citizenship: P.O. Address:

161c~6 Lake Jackson, Texas 77566T$ United States of America United States of America Same as Residence

sgnature Full Name: Resldence:

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city, state, ZIP:
Country: Cttizensh~p:

P.O. Address:

~hih-~a& L'ai 4523 Bermuda Drive Sugar Land. Texas 77479 T ' F United States of America United States of America Same aslResidence

4-73~
.

) . Addlt~onalw m r s ~ . . ds qna-ore, a r e attached
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EX. B PAGE 41
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Case 1:05-cv-00737-JJF
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Document 162-3
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Filed 09/04/2008
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Page 43 of 50

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,ON AND POWER OF ATTORNEf
ow named inventor, I My residence and Ci sought on the invention entitled: ted below my name My P 0. (mailing) address is thesame as my residence ,first and soleljoint inventor(s) of the subject matter which is embraced by and fokwhich a'patent

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IS
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FABRICATED ARTICLES MADE FROM ETHYLENE POLYMER BLENDS
is attached hereto (C- 40,121-G ).
was filed on as (C-). Application No. and was amended on
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nderstand the contents of the above identified specification, including the claims, as amended by any
6 to disclose to the U.S Patent and Trademark Office all information known t o me t o be material t d (b). I acknowledge the same duty of disclosure with respectto information which is first published or prior application claimed under paragraph (f) to the extent that the subject matter of any claim of this 3 application is not disclosed in the prior United States application. (e) Ihereby claim foreign priority benefits under Title 35, United StaJesCode 5 119 of any foreign application(s) for patent or inventor's certificate listed below and have also identified below any foreign application for patent or inventor's certificate having a filing date before that of the application on which priority is claimed: \ PRIOR FOREIGN APPLICATION(S) PRIORITY CLAIMED

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Number
J

,tountry

DaylMonthlYear I-{led

-?EFrnTT

h (f) Ihereby Claim the benefit y n d e r ~ i 35, United States Code 5 120of any United Statesapplications(s)listed below:

071776,130

October 15,1991
F~llng Date

Pending

Appl~cat~on serial NO.

3tatus (Patented, Pendlng, Aband

Ihereby appoint the following attorney($) andlor agent($) t o prosecute this application and t o transact all business in the Patent and Trademark . Office connected therewith. Address all correspondence to; THE DOW CHEMICAL COMPANY, Patent Dept., 8-1211 Freeport. TX 77541 and telephonic communications to the following: I (1) (2) (3) (4)

Stephen P. Krupp -L. w ayne white Glenn H. Korfhage Richard G. Waterman

(TEL.(409)238-2889

Reg. No. 34,366 Reg. No x3.413 Reg. No. 27,204 Reg. No. 20,128

this pppointment, including the right to delegate this appointment, shall also apply t o the same extent t o any proceedings establ 9 e d by the Patent Cooperation Treaty.
Ihereby declare that all statements made herein of my own knowledge are true and that all statements made on information and belief are believed t o be true; and further that these statements were made with the knowledge that willful false statements and the like so made are punishable by fine or imprisonment, or both under Title 18, United States Code 5 1001 and that such willful false statements may jeopardize the validity of the application or any patent issued thereon. Inventor(s): ~t

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Freeport, Texas 77541, U.S.A
day o f 19

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Freeport, Texas 77541, U.S.A.
day of I9

this Signature Full Name: Residence: City, State, Zip: Country: Citizenship: P.O. Address:

-

this Signature Full Name: Residence: City, State, Zip: Country: Citizenship: P.O. Address:

-

Pak-Wing Steve Chum 126 Juniper Street Lake Jackson, Texas 77566 United States of America United States of America Same as Residence

Ronald P. Markovich 1403 Bayou Oak Drive Friendswood, Texas 77546 United States of America United States of America Same as Residence

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Freeport, Texas 77541, U-S.A.
day o f 19
P

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Freeport, Texas 77541, U-S.A.
day of 19

1 B1

this Signature Full Name: Residence: City, State, Zip: country: Citizenship: P.O. Address:

this Signature ~ u lName: l Residence: city,itate, Zip: Country: Citizenship:
P.O. Address:

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1

George W. Knight 1618 North Road Lake Jackson, Texas 77566 United States of America United States of America Same as Residence

Shih-Yaw Cai 4523 Bermuda Drive Sugar Land, Texas 77479 United States of America United States of America Same a s R'esidence

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1
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R-10 88

( ) Addttional names and signatures are attached.

EX. B PAGE 42
>

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Case 1:05-cv-00737-JJF

Document 162-3

Filed 09/04/2008

Page 44 of 50

Case 1:05-cv-00737-JJF

Document 162-3

Filed 09/04/2008

Page 45 of 50

IN THC Document 162-3 D Case 1:05-cv-00737-JJF ~ N E T ESTATES PATENTAND TRADEMARK OFFICE Filed 09/04/2008 Page 46 of 50
Docket No. C40,121 -AU

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DavidWu

--

Mail Post Office t o Addressee'' service 'underq37 CFR 1 10 00 the #ate lndi~ated above and jr'addrvssed t o the Comrnlssioner o t rk* (patents and ~ r a d e ~ i ~ aWasbiruyt011,U C 20231

\ continuation ) divisional ) application under 37 CFR 1.60 and claiming benefit under 35 USC 120 o f pending prior application Serial No. 08378,998 filetl on January 27,1995 of Pak-Winq Steve Chum; Ronald P. Markovich; Geojqe W. Kn~qht, Sh~h-Yaw Lai for FABRICATEDARTICLES MADE FROM ETHYLENE POLYMER BLENDS J -

is is a request for filing a

-

1 2.

Enclosed isa copy of the prior application, Including the oath or declaration asoriginally filed Cancel in this application original clalrns of the prlor application before calculating the filing fee.

Total Claims 30 - 2 0 -Independent Claims 4 -3 -Multiple Dependent Claims Presented Total Fillng Fee

= =

10 1 --

x

-2 ? b O = $

-----

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recorded a t Reel No. 9. The inventorshlp of this appllcation 1 the same as that of the p r ~ ocopending U.S a p p l i c a t ~ o ~ ~ s r Fewer inventors are t o be named In this appllcatlon than Ir, the prior copending U.S. appl~cation Delete as ~nverrfor(s) t h ~ appllcatlon In s --- - -

-

--

10

The Power of Attorney In the prlor appltcatlon ~ s t o STEPHEN P. KRUPP, Req. No 34,366, L Wayne Wh~te, Req. No 2k4_1& Glenn H.Korfhaqe, Req No. 27,204; Richard G. Waterman, Req No 20,128 -Please address all commun~cat~ons _O.sborne K. McKlnney, 2301 Brazosport Blvd., B- 121 1; Freeport, Texas 77541to a. The power appears In the ortginal papers In the prior application b. The power does not appear In the orlglnal papers. A copy of the power In the prlor appllcation is enclosed c. Recognize as Associate Attorney Osborne K. McK~nnev w h o s e Registration NO IS P-40,084 --- and whose phone number IS (409) 238-7889

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,

11 C] A Preliminary Amendment IS enclosed (Clalmsadded by th~samendment have been properly numbered consecut~vely beginning w ~ t the number next foilow~ng hlghest numbered orig~nal h the clalm In the prlorappllcation ) 12

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13.
,

A new Dlsclosure Statement IS enclosed Applicant(s)' Dlsclosure Statement 1 as filed w ~ t h parent appllcatlon (copy attached) s the
I hereby ver~fy that the attached papers are t r ~ copy of prior applicat~on ~e Serlal No - 081378,998 as originally filed on January 27,1995 - -- , a l t h the exception that the dttorney's docket number in the I%er left-hend corner of each papes bas beer ddjusted ( ( 1 irflectthe instan4 aPpllcatlon
1

p e d decl