α-olefin interpolymers with improved molecular design for photovoltaic encapsulants

Abstract

A solution polymerization process for preparing ethylene / α-olefin / interpolymer, and an article comprising components formed from a composition containing the interpolymer. [Solution] A solution polymerization process for preparing ethylene / α-olefin / interpolymer comprises polymerizing a reaction mixture containing ethylene, α-olefin, a solvent, and a biphenylphenol metal complex selected from the following structures 1, in a single reactor at a reactor temperature of 150°C or higher. JPEG2026062729000023.jpg63170

Description

[Technical Field]

[0001] (Cross-reference of related applications) This application, dated December 26, 2019, is incorporated herein by reference in its entirety. We claim priority to international application No. CN2019 / 128574 filed in [location]. [Background technology]

[0002] Polymers designed for photovoltaic encapsulants must meet many requirements. To prevent movement of electrical components and wiring during testing and use, the polymer material is rated for temperatures up to 85°C. It is necessary to ensure that it does not flow significantly at this temperature. One way to achieve this is, This includes a semicrystalline polymer having a melting point above this temperature. However, high light Other requirements for sealing materials, such as transparency and low modulus of elasticity, are optimized with low-crystallinity polymers. To balance these requirements, typically, ethylene-vinyl acetate copolymers are used. (ethylene-vinyl acetate copolymer, EVA) or polyolefin elastomer (poly Low-crystallinity polymers such as olefin elastomers (POE) are used in peroxide-based reactive curing processes. It is used in conjunction with the packaging. Low crystallinity polymers provide high transparency and low modulus of elasticity. However, the curing package allows the polymer to form a network, providing mechanical stability at high temperatures. This promotes the crosslinking reaction. This crosslinking reaction is typically carried out in a module at 150°C. It occurs during lamination.

[0003] The peroxide curing package contains peroxides that decompose and form in the extruder. To prevent the crosslinking reaction from starting, the film extrusion process needs to be carried out at a low temperature. Therefore, it leads to additional design inconsistencies. The heat generated during extrusion is related to the extrusion rate and polymer viscosity. High viscosity and high extrusion rate generate more heat. Therefore, peroxide curing occurs. To extrude the composition, it is preferable to extrude the low-viscosity resin at a low speed. However, Furthermore, low extrusion rates are economically disadvantageous, and low viscosity is typically achieved through the use of low molecular weight resins. This is achieved. Typically, low molecular weight resins cannot be efficiently crosslinked, and the required level of crosslinking is not achieved. To achieve this, in the module stacking process, the peroxide curing package is more efficient. It requires a larger filling volume or a longer time. All of these solutions are costly and non It is efficient.

[0004] Compared to conventional polymers used in photovoltaic encapsulants, it can be extruded at high speed. There is a need for a new polymer that is highly crosslinkable. European Patent No. 295815 Document 1(B1) discloses a resin composition for solar cell encapsulants, which has good crosslinking and good It is disclosed as having heat resistance and good transparency. The resin composition is related to the following: It contains an ethylene / α-olefin copolymer satisfying N×V≧10, where N is co This is the branching number derived from the monomer, where V is the total number of vinyl and vinylidene molecules in the copolymer. There is (see, for example, paragraphs

[0030] and

[0031] ). Here, V is 0.17 or less. See above. Also, please refer to Patent Publication No. 2012009688(A) (machine translation). This is because it is 0.22 unsaturated (vinyl, vinylidene, cis and trans vinylene, trisubstituted). Total amount of vinylene, density of 0.860-0.920 g / cc, and Mz / M of 8.0 or less. Disclosed: A solar encapsulation composition containing an ethylene / α-olefin copolymer having n. An additional polymer composition for solar encapsulants is described in the following reference: European Patent No. 26 37217(B1) (Partially, MFR less than 2-10, 0.865-0.884g / It contains a density of cc and a Shore A hardness of 60-85, and its MWD can be 1.2-3.5. (a composition containing ethylene / α-olefin copolymer), and U.S. 85810 No. 94 (partially, density less than approximately 0.90 g / cc, melting point less than approximately 95°C, and approximately 150 (A composition containing a polyolefin copolymer with a 2% secant modulus of less than megapascals) This is disclosed in [the document]. However, these references do not achieve high extrusion speed and high crosslinking degree. This does not promote new resin designs for the purpose of promoting high extrusion speed and high crosslinking degree. The need for such compositions still exists. This need is satisfied by the present invention. It was done. [Overview of the project]

[0005] The following characteristics: a) Total unsaturation of 0.30 or more / 1000C, b) Molecular weight distribution (MWD) of 3.0 or less, c) TGIC spread parameter B of 8.0 or less 1 / 4 , containing ethylene / α-olefin A composition containing an internomer.

[0006] In a solution polymerization process for preparing ethylene / α-olefin / interpolymers In this process, in a single reactor, at a reactor temperature of 150°C or higher, ethylene Polymerization of a reaction mixture containing an α-olefin, a solvent, and a metal complex selected from a) below This includes doing a) Biphenylphenol metal complex selected from the following structure 1: [Chemical formula] M is Zr or Hf, and the metal is in an oxidation state of +2, +3, or +4, n is 0, 1, or 2, When n is 1, X is a monodentate ligand or a bidentate ligand, When n is 2, each X is an independently selected monodentate ligand, The metal complex is overall charge-neutral, -Z 1 - and -Z 2 Each of - is independently selected from -O-, -S-, -N(R N ), or -P(R P ), R 1 and R 8 are independently -H, (C1-C 40 )-hydrocarbyl, (C1-C 40 )heterohydrocarbyl, -Si(R C )3, -Ge(R C )3, -P(R P )2, -N(R N ), -OR C -SR C -NO2, -CN, -CF3, R C S(O)-, R C S(O)2-, (R C )2C=N-, R C C(O)O-, R C OC(O)-, R C C (O)N(R)-, (R C )2NC(O)-, halogen, a radical having formula (I), a radical having formula (II), and a radical having formula (III) and is selected from the group consisting of , [Chemical formula] wherein R 31~35 , R41~48 , and R 51~59 Each of them is independent, (C1 ~C 40 ) Hydrocarbyl, (C1~C 40 ) Heterohydrocarbyl, -Si(R C )3 ,-Ge(R C )3, -P(R P )2, -N(R N )2, -N=CHR C , -OR C ,- SR C -NO2, -CN, -CF3, R C S(O)-, R C S(O)2-, (R C )2 C=N-, R C C(O)O-, R C OC(O)-, R C C(O)N(R N )-, (R C ) Selected from 2NC(O)-, halogen, or -H, R 2~7 , R 9~16 Each of these is independent of (C1~C 40 ) Hydrocarbyl, (C 1~C40) Heterohydrocarbyl, -Si(R C )3, -Ge(R C )3, -P(R P )2, -N(R N )2, -N=CHR C , -OR C , -SR C -NO2, -CN, -C F3, R C S(O)-, R C S(O)2-, (R C )2C=N-, R C C(O)O-, R C OC(O)-, R C C(O)N(R N )-, (R C )2NC(O)-, halogen, or - Selected from H, L is (C1~C 40 ) Hydrocarbylene or (C1~C 40 ) Heterohydrocarb It is Ren, (C1~C 40 ) Hydrocarbylene has two Z groups (L) in structure 1. A portion containing a linker backbone of 1 to 10 carbon atoms that connects (the combined) Having or (C1~C 40 ) Heterohydrocarbylene has two Z in structure 1 It has a portion containing a linker main chain of 1 to 10 atoms that connects the groups, (C1 to C 40 ) 1 to 10 atoms of heterohydrocarbylene linker backbone Each of the atoms is independently a carbon atom or a heteroatomic group, and each heteroatomic group is independently Then, O, S, S(O), S(O)2, Si(R C )2, Ge(R C )2, P(R C ), or N(R C ) and each R in structure 1 C , R P , and R N (C1~ C 30 ) Hydrocarbyl, (C1~C 30 ) Heterohydrocarbyl, or -H, soluble Liquid polymerization process.

[0007] TGIC spreading parameters of a polymer composition containing one or more olefin polymers Ta B 1 / x A method for making a determination, the method comprising the following steps: a) A step of dissolving the polymer composition in an organic solvent to form a polymer solution, b) Add at least a portion of the polymer solution to a column containing a support material including graphite. The injection step, c) A step of cooling the support material at a rate of 0.1°C / min or more. d) Increase the temperature of the support material to elute the polymer(s) of the polymer composition. Steps e) Step to generate a "dwi / dT vs temperature" profile, f) For the maximum height of the profile (dwi / dTi vs temperature), 1 / x of the maximum height Steps to calculate the width of the profile at (x>1), g) A step to determine the temperature (Tp) at the maximum height of the profile, h) Based on the EICOSANE / iPP / HDPE standard, (at an elution temperature of 150.0°C) Calculate the HDPE peak width (peak width at 1 / x) at 1 / x of the HDPE peak height. The steps are as follows, and the reference is analyzed by TGIC according to steps a) to g). The calculation step, i)B 1 / x The following formula:

number

[0008] [Figure 1] This graph shows the extrapolation of elution temperature for TGIC temperature calibration. The solid line represents experimental data, and the dashed line represents the extrapolation of elution temperature for two isothermal steps. [Figure 2] This is a TGIC chromatogram of an EICOSANE / iPP / HDPE mixture. [Figure 3] This graph shows the correlation between the elution peak temperature (Tp) of ethylene-octene copolymer and the weight percentage of octene. [Figure 4] This is a graph of the TGIC profile of the POE (POE A) of the present invention. [Figure 5] This is a graph of the TGIC profile for comparative POE (POE C). [Modes for carrying out the invention]

[0009] Ethylene / α-olefin / inter - A polymer design was discovered. Higher vinyl fraction in total unsaturated polymers and in interpolymers. It was also found that the narrow comonomer distribution provides improved adhesion to glass.

[0010] As mentioned above, the following characteristics: a) Total unsaturation of 0.30 or more / 1000C, b) Molecular weight distribution (MWD) of 3.0 or less, c) TGIC spread parameter B of 8.0 or less 1 / 4 , containing ethylene / α-olefin A composition containing an internomer is provided.

[0011] The above compositions include combinations of two or more embodiments as described herein. Obtain. Ethylene / α-olefin interpolymers are two such as those described herein. This may include combinations of the above embodiments.

[0012] The above TGIC spread parameter B 1 / 4 is ethylene / α-olefin interpoly This is an indicator of respiration in the comonomer distribution of Mer. Smaller B 1 / 4 The value is a narrower Komonoma —Shows the distribution. One embodiment, or two or more embodiments each described herein. In combination, the TGIC spread parameter B 1 / 4 is 7.5 or less, or 7.0 or less. or 6.5 or less, or 6.0 or less, or 5.5 or less, or 5.0 or less, or 4.8 or less, Or 4.6 or less, or 4.4 or less, or 4.2 or less, or 4.0 or less, or 3.8 or less Yes. One embodiment, or a combination of two or more embodiments described herein. So, the TGIC spread parameter B 1 / 4 is 1.5 or higher, or 2.0 or higher, or 2. 2 or higher, or 2.4 or higher, or 2.6 or higher, or 2.8 or higher, or 3.0 or higher, or 3. It is 2 or greater.

[0013] One embodiment, or a combination of two or more embodiments, each described herein. Therefore, the ethylene / α-olefin interpolymer is 0.860 g / cc or more, or 0. 861 g / cc or more, or 0.862 g / cc or more, or 0.863 g / cc or more, 0.864 g / cc or more, or 0.865 g / cc or more, or 0.866 g / cc or more, Or 0.867 g / cc or more, or 0.868 g / cc or more, or 0.869 g / cc or less Above, or 0.870 g / cc or more (1 cc = 1 cm³) 3 ) has a density of ). In one embodiment, Each of the combinations of two or more embodiments described herein is ethylene / α -Olefin interpolymers are 0.900 g / cc or less, or 0.890 g / cc or less. Below, or 0.888 g / cc or less, or 0.886 g / cc or less, or 0.885 g / cc c or less, or 0.884 g / cc or less, or 0.883 g / cc or less, or 0.882 g Having a density of 0.880 g / cc or less, or 0.878 g / cc or less. .

[0014] One embodiment, or a combination of two or more embodiments, each described herein. Therefore, the ethylene / α-olefin interpolymer is 0.32 or higher, or 0.35 or higher. , or 0.40 or higher, or 0.45 or higher, or 0.50 or higher, or 0.52 or higher, or 0 It has a total unsaturation / 1000C of 0.54 or more, or 0.56 or more. In one embodiment, or in each combination of two or more embodiments described herein where each is a combination of two or more embodiments described herein, the ethylene / α-ole fin interpolymer has a total unsaturation / 1000C of 1.00 or less, or 0.95 or less, or 0.90 or less, or 0.85 or less, or 0.80 or less, or 0.78 or less, or 0.76 or less, or 0.74 or less, or 072 or less, or 0.70 or less.

[0015] In one embodiment, or in each combination of two or more embodiments described herein the ethylene / α-olefin interpolymer has a molecular weight distribution (MWD = Mw / Mn) of 1.6 or more, or 1.7 or more, or 1.8 or more, or 1.9 or more, or 2.0 or more. In one embodiment, or in each combination of two or more embodiments described herein the ethylene / α-olefin interpolymer has a molecular weight distribution MWD of 2.9 or less, or 2.8 or less , or 2.7 or less, or 2.6 or less, or 2.5 or less, or 2.4 or less, or 2.3 or less , or 2.2 or less.

[0016] In one embodiment, or in each combination of two or more embodiments described herein the interpolymer has [(vinyl / 1000C) * (Mn)] of 5.0×10 3 (g / mol) or more, or 6.0×10 3 (g / mol) or more, 7.0×10 3 (g / m ol) or more, 7.5×10 3 (g / mol) or more, or 8.0×10 3 (g / mol) or more, or 8.5×10 3 (g / mol) or more, or 9.0×10 3(g / mol) or more, or 9.5×10 3 (g / mol) or more, or 10×10 3 (g / mol) or more and further contains a product. In one embodiment, or a combination of two or more embodiments described herein ((vinyl / 1000C) * (Mn)) is 3 0×10 3 (g / mol) or less, or 20×10 3 (g / mol) or less,), or 18× 10 3 (g / mol) or less, or 16×10 3 (g / mol) or less, or 14×10 3 ( g / mol) or less, or 12×10 3 (g / mol) or less and further contains a product.

[0017] In one embodiment, or a combination of two or more embodiments described herein ((vinyl / 1000C) / (vinylidene / 1000C)) ratio is 2.0 or more, or 2.2 or more, or 2.4 or more, or 2.6 or more, or 2.8 or more, or 3.0 or more, or 3.1 or more, or 3.2 or more, or 3.3 or more, or 3.4 or more and further includes that. In one embodiment, or a combination of two or more embodiments described herein, the interpolymer [(vinyl / 1000C) / (vinylidene / 1000C)] ratio is 6.0 or less, or 5.5 or less, or 5.0 or less, or 4. 8 or less, or 4.6 or less, or 4.4 or less, or 4.2 or less, or 4.0 or less, or 3. 8 or less and further includes that.

[0018] In one embodiment, or a combination of two or more embodiments described herein So, the ethylene / α-olefin interpolymer is 50% or more, or 52% or more, It contains 54% or more, or 56%, or 58% or more, or 60% or more, or 62% or more vinyl. Further includes %. Vinyl % = [(Vinyl / 1000C) / (Total Unsaturated / 1000C)] × 1 00.

[0019] One embodiment, or a combination of two or more embodiments, each described herein. The composition further comprises a peroxide and a silane coupling agent. One embodiment, or In each combination of two or more embodiments described herein, the composition is crosslinked. It also contains auxiliary agents.

[0020] Any one embodiment, or any combination of two or more embodiments described herein. An article comprising at least one component formed from a composite composition is also provided. In the form of implementation, or in combination of two or more embodiments described herein, the object The product is a film. One embodiment, or two or more embodiments, each described herein. In this combination of installation forms, the item is a solar cell module.

[0021] Ethylene / α-olefin interpolymers are polymerized from ethylene and α-olefins. Contains fins. α-olefins can be either aliphatic or aromatic compounds. α- The olefin is preferably C3-C 20 Aliphatic compounds, preferably C3-C 16 Aliphatization A mixture, and more preferably C3~C 10 It is an aliphatic compound. Preferred C3-C 10 fat Examples of group α-olefins include propylene, 1-butene, 1-hexene, 1-octene, and Examples include 1-decene, and more preferably 1-octene.

[0022] The peroxide (containing at least one "-OO-" group) is preferably a Peroxides, for example, t-butylperoxy-2-ethylhexyl carbonate, di -Butylbutylperoxide, t-butylcumylperoxide, dicumylperoxide , 2,5-dimethyl-2,5-di-(t-butylperoxy)hexane, di-(t-butyl -peroxy-isopropyl)benzene, t-butylperoxybenzoate, 1,1- di-(t-butylperoxy)-3,3,5-trimethylcyclohexane, 2,5-di Methyl-2,5-di(t-amylperoxy)-hexane,2,5-dimethyl-2,5- Di(t-butyl-peroxy)hexyn-3,2,5-dimethyl-2,5-di(t-amide) Luperoxy)hexine-3, di-t-amylperoxide, 1,3-dimethyl-3-( t-butyl-peroxy)butanol, 1,3-dimethyl-3-(t-amylperoxy )Butanol, and mixtures of two or more initiators thereof, for example, Ak zoNobel's TRIGONOX peroxide, ARKEMA's LUPEROX peroxide Please refer to Luoxide.

[0023] Examples of silane coupling agents include vinyltrimethoxysilane and 3-(trimethoxy Examples include, but are not limited to, silyl)propyl methacrylate as a crosslinking aid. Triallyl cyanurate, triallyl phosphate, triallyl isocyanurate , and 1,3,5,7-tetravinyl-1,3,5,7-tetramethylcyclotetrasil Examples include, but are not limited to, xanes. The compositions of the present invention also include UV stabilizers and acids. It may contain one or more additives, such as anti-corrosion agents and combinations thereof.

[0024] One embodiment, or a combination of two or more embodiments, each described herein. The composition of the present invention is characterized by the type and / or amount of monomer(s), Mn, Mw, M z, MWD, V0.1, V100, RR(V0.1 / V100), or any combination thereof. In one or more characteristics, such as intercombination, ethylene / α-olefin interpolymer It further contains thermoplastic polymers different from those mentioned above. Examples of polymers include ethylene-based polymers and pro Examples include pyrene-based polymers and olefin multiblock interpolymers, The following are not the only suitable ethylene polymers. Linear low-density polyethylene (LLDPE), very low-density polyethylene (LLDPE) Ultra-low density polyethylene (VLDPE), ultra-low density polyethylene Hylene (ULDPE), homogeneously branched linear ethylene polymers, and homogeneously branched A substantially linear ethylene polymer (i.e., a homogeneously branched long-chain branched ethylene polymer) Examples of propylene polymers include, but are not limited to, rimers. Examples include polypropylene homopolymers and propylene / ethylene copolymers.

[0025] Solution polymerization processes for preparing ethylene / α-olefin / interpolymers are also available. The process involves providing ethylene in a single reactor at a reactor temperature of 150°C or higher. , α-olefin, solvent, and Summary of the Invention (SOI) A reaction mixture containing a metal complex selected from Structure 1, as described below, is polymerized. This includes.

[0026] The process of the present invention is a combination of two or more embodiments as described herein. It may include two or more biphenylphenol metal complexes as described herein. This may include combinations of embodiments. When used herein, R1 = R 1 , R²=R 2 , R3=R 3 And so on. Also, "a(1) to a(n)" represents consecutive numbers, R a(1) ~R a(n) This notation is R a(1) , R a(2) , R a(3) ... R a(n) This refers to R. 31 ~R 35 R 31 , R 32 , R 33 , R 34 , R 3 5 It refers to R 51 ~R 59 R 51 , R 52 , R 53 , R 54 , R 55 , R 56 , R 5 7 , R 58 , R 59 This refers to... In each of equations (I) to (III), the wavy line indicates the respective equation ( R 1 or R 8 This shows the adhesion (bonding) between the base and the remainder of the biphenylphenyl metal complex.

[0027] One embodiment, or a combination of two or more embodiments, each described herein. Now, regarding structure 1, L is -(CH2) n -(where n=2~4 in the formula), -CH2 C(R a R b )CH2-(wherein, R a and R b Each of them is independent, (C1~C 40 ) Hydrocarbyl, (C1~C 40 )heterohydrocarbyl, or -H), or -C H2Ge(R D )2CH2- or -CH2Si(R D )2CH2-(in the formula, each R D German Standing, -H, (C1~C 40 ) Hydrocarbyl, (C1~C 40 ) Heterohydrocarb Ru, -Si(R C )3, -Ge(R C )3, -P(R P )2, -N(R N )2, -OR C , -SR C -NO2, -CN, -CF3, R C S(O)-, R C S(O)2-, (R C )2C=N-, R C C(O)O-, R C OC(O)-, R C C(O)N(R N )-, and (R N Selected from the group consisting of )2NC(O)-, each R in structure 1 C , R P , and R N teeth , independently, (C1~C 30 ) Hydrocarbyl, (C1~C 30 ) Heterohydrocarbyl It is either , or -H.

[0028] One embodiment, or a combination of two or more embodiments as each described herein. In the combination, for structure 1, L is -CH2C(R a R b )CH2-(wherein, R a and R b Each of them is independent, (C1~C 40 ) Hydrocarbyl, (C1~C 40 ) heterozygous Hydrocarbyl, or -H), or -CH2Ge(R D )2CH2- or -C H2Si(R D )2CH2-(in the formula, each R D These are independently -H, (C1~C 40 ) Hidden Locarvir, and (C1~C 40 (Selected from the group consisting of heterohydrocarbyls) It is one of the two.

[0029] One embodiment, or a combination of two or more embodiments, each described herein. Now, regarding structure 1, -Z 1 - and -Z 2 Each of the - is -O-.

[0030] One embodiment, or a combination of two or more embodiments, each described herein. Now, regarding structure 1, R 1 and R 8 These are identical, and radicals having formula (I), formula ( From the group consisting of radicals having formula (II) and radicals having formula (III), further, formula ( Selected from radicals having (II)

[0031] One embodiment, or a combination of two or more embodiments, each described herein. Now, for structure 1, n=2, each X is the same, and it is an unsubstituted alkyl group.

[0032] One embodiment, or a combination of two or more embodiments, each described herein. So, the reaction mixture consists of co-catalyst-1 containing borate and co-catalyst-2 containing almoxane. It also includes.

[0033] One embodiment, or a combination of two or more embodiments, each described herein. So, the process is at 155°C or above, or 160°C or above, or 165°C or above, or 170°C. Above, or 175°C or above, or 180°C or above, or 185°C or above, or 186°C or above, This is done at a reactor temperature of 187°C, or 188°C or higher, or 189°C or higher, 2.5 × 10 6 The above, or 2.6 × 10 6 The above, or 2.8 × 10 6 Above, or 3.0× 10 6 The above, or 3.2 × 10 6 The above, or 3.4 × 10 6 The above, or 3.6 × 10 6 Below Top, or 3.7 × 10 6 The above, or 3.8 × 10 6 The above, or 3.9 × 10 6 The above, or 4.0×10 6 The above, or 4.1 × 10 6 The above, or 4.2 × 10 6 The overall catalyst It has an efficiency of [(grams of interpolymer) per (grams of total catalyst metal)].

[0034] One embodiment, or a combination of two or more embodiments, each described herein. So, the process is 0.860~0.900 g / cc, or 0.865~0.890 g / cc, or 0.868~0.880g / cc (1cc = 1cm³) 3 ) ethylene / α-ole Fin / interpolymer density: 2.5 × 10 6 The above, or 2.6 × 10 6 The above, or 2.8 × 10 6 Above, or 3.0 × 10 6 The above, or 3.2 × 10 6 Above, or 3.4× 10 6 The above, or 3.6 × 10 6 The above, or 3.7 × 10 6 The above, or 3.8 × 10 6 Below Top, or 3.9 × 10 6 Above, or 4.0 × 10 6 The above, or 4.1 × 10 6 The above, or 4.2 × 10 6 The overall catalytic efficiency [(total catalyst metal grams) per (interpoly It has Margram.

[0035] One embodiment, or a combination of two or more embodiments, each described herein. So, the process is at 155°C or above, or 160°C or above, or 165°C or above, or 170°C. Above, or 175°C or above, or 180°C or above, or 185°C or above, or 186°C or above, This is achieved at reactor temperatures of 187°C, or 188°C or higher, or 189°C or higher, or 190°C or higher. This is carried out in one embodiment, or in combination of two or more embodiments described herein. In combination, the process is performed at a temperature of 250°C or below, or 240°C or below, or 230°C or below. The process is carried out at a reactor temperature of 20°C or below, or 210°C or below, or 200°C or below.

[0036] The term "substituent" refers to a bond to a carbon or heteroatom in the corresponding unsubstituted compound. A substituent (R) on the hydrogen atom (-H) S This refers to substitution by "R". S The notation " is This refers to a chemical group containing a heteroatom or at least one heteroatom. (The term "substitution" is used.) This includes at least one water atom bonded to a carbon or heteroatom of the corresponding unsubstituted compound. Elementary atom (-H) is a substituent (R s This means that it will be replaced by ).

[0037] The term "heteroatom" refers to an atom other than hydrogen or carbon. The term refers to a heteroatom or a chemical group containing one or more heteroatoms. Examples of bases include O, S, S(O), and S(O). 2、 Si(R C ) 3、 P(R P )2, N( R N )2, -N=C(R C )2, -Ge(R C )2-, or -Si(R C )2-(in the formula, Each R C and each R P These are independently, non-substitutable (C1~C 30 ) Hydrocarbyl, or H , each R N is non-substitutable (C1~C 30 (Hydrocarbyl is one example), but these include Not limited.

[0038] The term "-H" refers to hydrogen or a hydrogen radical that is covalently bonded to another atom. "Hydrogen", H, and "-H" are interchangeable and, unless otherwise specified, represent the same thing. It means.

[0039] (C1~C 40 The term "hydrocarbyl" refers to a type of carbonized water with 1 to 40 carbon atoms. "(C1~C)" means elementary radicals. 40 The term "hydrocarbylene" is used in 1 to 40 units. It means a hydrocarbon diradical of a carbon atom, and each hydrocarbon radical and each hydrocarbon diradical The term "ru" refers to aromatic or non-aromatic, saturated or unsaturated, linear or branched, and cyclic (monocyclic and polycyclic) structures. (including condensed and non-condensed polycyclic compounds, including bicyclic compounds, with three or more carbon atoms) or acyclic compounds. , unsubstituted, or one or more R S It has been replaced by.

[0040] The term "heterohydrocarbon" refers to a compound in which one or more carbon atoms are replaced by heteroatoms. It refers to a molecule or molecular skeleton. (C1~C 40 The term "heterohydrocarbyl" is, This refers to heterohydrocarbon radicals consisting of 1 to 40 carbon atoms, or "(C1~C 40 ) Heterohy The term "drocarbylene" refers to a heterohydrocarbon diradical with 1 to 40 carbon atoms. Each heterohydrocarbon has one or more heteroatoms. The diradical is located on a carbon atom or heteroatom, and the diradical of heterohydrocarbyl is ( 1) one or two carbon atoms, (2) one or two heteroatoms, or (3) one It can be on one carbon atom and one heteroatom. Each (C1~C 40 ) Heterohydrocal Building and (C1~C 40 ) Heterohydrocarbylene is unsubstituted or (one or more R S by Substitution, aromatic or non-aromatic, saturated or unsaturated, linear or branched, cyclic (monocyclic and It may be polycyclic, condensed, or acyclic (including polycyclic and non-condensed polycyclic forms).

[0041] The terms "halogen atom" or "halogen" refer to fluorine atoms (F), chlorine atoms (C) l) refers to a radical of a bromine atom (Br) or an iodine atom (I). "Halogen The term "fluoride (F-), chloride (Cl-), bromide (Br-), or iodide" refers to fluoride (F-), chloride (Cl-), bromide (Br-), or iodide. This refers to the anionic form of a halogen atom, such as (I-).

[0042] TGIC spreading parameters of a polymer composition containing one or more olefin polymers Ta B 1 / x A method for determining the SOI, the method comprising the steps described above. A method is also provided. This method is a combination of two or more embodiments as described herein. It may include combinations.

[0043] One embodiment, or a combination of two or more embodiments, each described herein. Then, the composition shall be based on the weight of the composition, with 50% or more by weight, or 60% or more by weight, 70% or more by weight, or 80% or more by weight, or 85% or more by weight of one or more olefin-based polymers It contains rimer, and further 50% or more by weight, or 60% or more by weight, or 70% or more by weight, or 8 One olefin polymer in an amount of 0% or more by weight, or 85% or more by weight, and further ethylene / α- Contains olefin interpolymers.

[0044] One embodiment, or a combination of two or more embodiments, each described herein. Then, the composition shall be based on the weight of the composition, with 90% or more by weight, or 92% or more by weight, One of the following: 94% by weight or more, or 96% by weight or more, or 98% by weight or more, or 99% by weight or more. The above olefin polymers are included, and further 90% or more by weight, or 92% or more by weight, or 9 One of the following: 4% by weight or more, or 96% by weight or more, or 98% by weight or more, or 99% by weight or more It contains olefin polymers, and further, ethylene / α-olefin interpolymers.

[0045] One embodiment, or a combination of two or more embodiments, each described herein. In this example, the composition contains only one olefin polymer. In a further embodiment, olefin The olefin polymer is an ethylene / α-olefin interpolymer.

[0046] One embodiment, or a combination of two or more embodiments, each described herein. Therefore, the support material shall be 10% or more by weight, or 20% or more by weight, based on the weight of the support material. or 30% by weight or more, or 40% by weight or more, or 50% by weight or more, or 60% by weight or more, Or it contains 70% or more by weight of graphite, or 80% or more by weight of graphite, or 85% or more by weight of graphite.

[0047] One embodiment, or a combination of two or more embodiments, each described herein. Therefore, the support material shall be 90% or more by weight, or 92% or more by weight, based on the weight of the support material. Or 94% or more by weight, or 96% or more by weight, or 98% or more by weight, or 99% or more by weight Contains graphite.

[0048] definition Unless otherwise stated, the context implicitly or conventionally in the relevant technical field is To the extent that, all parts and percentages are based on weight, and all test methods are as of the filing date of this disclosure. This is the current version at that time.

[0049] As used herein, the term “composition” means the composition and the materials of the composition. The mixture of materials includes reaction products and decomposition products formed from any reaction. Substances or decomposition products are also typically present in trace or residual amounts.

[0050] As used herein, the term "polymer" refers to the same or different types of polymers. Refers to a polymer compound prepared by polymerizing monomers. Thus, the polymer The general term "polymer" includes the term "homopolymer" (under the understanding that a polymer prepared from only one type of monomer can incorporate trace amounts of impurities) and the term "interpolymer" as defined below in this specification. Trace amounts of impurities such as catalyst residues can be incorporated into and / or within the polymer. Typically, the polymer is stabilized with very small amounts (in the "ppm" range) of one or more stabilizers.

[0051] As used herein, the term "interpolymer" refers to a polymer prepared by polymerizing at least two different types of monomers. Thus, the term "interpolymer" includes the term "copolymer" (used to refer to a polymer prepared from two different types of monomers) and polymers prepared from more than two different types of monomers.

[0052] As used herein, the term "olefin-based polymer" refers to a polymer that contains 50 wt% or more (based on the weight of the polymer) of an olefin such as ethylene or propylene in polymerized form and optionally contains one or more comonomers.

[0053] As used herein, the term "propylene-based polymer" refers to a polymer that contains more than half weight percent of propylene in polymerized form and optionally can contain one or more comonomers.

[0054] As used herein, the term "ethylene polymer" refers to a polymer that, in polymerized form, contains 50 weight percent or a majority weight percent of ethylene ( based on the weight of the polymer) and optionally may contain one or more comonomers.

[0055] As used herein, the term "ethylene / α-olefin interpolymer" refers to a random interpolymer that, in polymerized form, contains 50 weight percent or a majority weight percent of ethylene ( based on the weight of the interpolymer) and an α-olefin.

[0056] As used herein, the term "ethylene / α-olefin copolymer" refers to a random copolymer that, in polymerized form, contains, as only two monomer types, 50 weight percent or a majority amount of an ethylene monomer ( based on the weight of the copolymer) and an α-olefin.

[0057] As used herein, the term "solution polymerization" refers to a polymerization process in which monomers (plural possible) as well as the polymer being produced are dissolved in a polymerization solvent. In one embodiment, the reactor pressure is 1000 psig or less.

[0058] As used herein, the term "reaction mixture" refers to a mixture that contains one or more monomer types, a solvent, and a metal complex. Typically, the reaction mixture also contains one or more cocatalysts and hydrogen (H2).

[0059] As used herein with respect to a polymerization process, the term "overall catalyst efficiency (units of 10≦6 g of polymer per g of total catalyst metal)" refers to the amount of polymer produced per gram of total catalyst metal in the same polymerization process (or polymerization run The total amount of catalyst metals used in the process (e.g., metals from one or more metal complexes) The amount formed during the polymerization process (or polymerization run), divided by the supply rate (e.g., lb / hour). This refers to the rate at which the polymer is produced (e.g., pounds / hour). Typically, polymerization occurs in a steady state. It is Rothes.

[0060] As used herein, the term "silane coupling agent" means at least 1 One "Si" atom, and at least one "-CH2-" group, and / or at least one This refers to a compound containing the "-CH3" group, which acts as a bridge between two materials, for example, poly A chemical bond is formed between the polymer and the inorganic material.

[0061] As used herein, the term "solar cell (or photovoltaic cell)" means solar This refers to a device that converts light irradiation into electricity. Solar cells are typically presented in an array pattern. It will be done.

[0062] When used herein, "solar cell module (or solar panel or solar) The term "module" refers to a photovoltaic panel comprising an assembly of solar cells.

[0063] As used herein, "laminating" and "lamination" are used interchangeably. The term and similar terms refer to multiple layered materials that are subjected to heat and pressure, as well as optional vacuum. This refers to processes that are combined under certain conditions.

[0064] The usages of "comprising," "including," and "having" Words and their derivatives are arbitrary, regardless of whether they are specifically disclosed or not. It is not intended to exclude the existence of additional components, steps, or procedures. For the sake of avoiding ambiguity, all compositions claimed through the use of the term "comprising" shall, whether polymers or not, include any additional additives, adjuvants, or compounds, unless there is a contrary description. In contrast, the term "consisting essentially of" excludes those that are not essential for operation and excludes any other components, steps, or procedures from the scope of any subsequent detailed description. The term "consisting of" excludes any component, step, or procedure that is not specifically specified or enumerated.

[0065] Enumerating some characteristics of compositions A] The following characteristics: a) Total unsaturation of 0.30 or more per 1000C, b) Molecular weight distribution (MWD) of 3.0 or less, c) TGIC spread parameter B of 8.0 or less 1 / 4 , an ethylene / α-ole fin interpolymer, a composition. B] The ethylene / α-olefin interpolymer has a density of 0.860 g / cc or more, or 0.861 g / cc or more, or 0.862 g / cc or more, or 0.863 g / cc or more, or 0.864 g / cc or more, or 0.865 g / cc or more, or 0.866 g / cc or more, or 0.867 g / cc or more, or 0.868 g / cc or more, or 0.869 g / c c or more, or 0.870 g / cc or more (1 cc = 1 cm 3 ), the composition described in A] above. C] The ethylene / α-olefin interpolymer has a density of 0.900 g / cc or less, or 0.890 g / cc or less, or 0.888 g / cc or less, or 0.886 g / cc or less, Or 0.885 g / cc or less, or 0.884 g / cc or less, or 0.883 g / cc or less Below, or 0.882 g / cc or less, or 0.880 g / cc or less, or 0.878 g / cc The composition according to A] or B] above, having a density of c or less. D] Ethylene / α-olefin interpolymer is 0.32 or higher, or 0.35 or lower. Above, or 0.40 or above, or 0.45 or above, or 0.50 or above, or 0.52 or above, Having a total unsaturated / 1000C of 0.54 or more, or 0.56 or more, the above A]~C](A A composition as described in any one of the following (from C to C). E] Ethylene / α-olefin interpolymer is 1.00 or less, or 0.95 or less. Below, or 0.90 or less, or 0.85 or less, or 0.80 or less, or 0.78 or less, Total unsaturated ratio of 0.76 or less, or 0.74 or less, or 0.72 or less, or 0.70 or less / 10 A composition according to any one of A] to D] above, having 00C. F] Ethylene / α-olefin interpolymer, 50% or more, or 52% or more. Or 54% or more, or 56%, or 58% or more, or 60% or more, or 62% or more vinyl A composition according to any one of A] to E] above, further comprising %. G] Ethylene / α-olefin interpolymer is 100% or less, or 95% or less. , or 90% or less, or 85% or less, or 80% or less, or less, or 78% or 76% or less, Or 74% or less, or 72% or less, or 70% or less, or 68% or less, or 66% or less A composition according to any one of A] to F] above, further comprising % vinyl. H]Ethylene / α-olefin interpolymer, [(vinyl / 1000C) * ( Mn) is 5.0 × 10 3 (g / mol) or more, or 6.0 × 10⁻⁶3 (g / mol) or less Top, 7.0×10 3 (g / mol) or more, 7.5x10 3 (g / mol) or more, or 8. 0 x 10 3 (g / mol) or more, or 8.5 × 10⁻⁶ 3 (g / mol) or more, or 9.0 × 10 3 (g / mol) or more, or 9.5 × 10⁻⁶ 3 (g / mol) or more, or 10 × 10 3 The set according to any one of A] to G] above further comprises a product having a concentration of (g / mol) or more. Finished product. I] Ethylene / α-olefin interpolymer, [(vinyl / 1000C) * ( Mn) is 30×10 3 (g / mol) or less, or 20 × 10 3 (g / mol) or less, ), or 18×10 3 (g / mol) or less, or 16 × 10 3 (g / mol) or less, 14×10 3 (g / mol) or less, or 12 × 10 3 Products that are less than or equal to (g / mol) Furthermore, the composition described in any one of A] to H] above. J] Ethylene / α-olefin interpolymer, [(vinyl / 1000C) / ( The ratio of vinylidene / 1000C is 2.0 or higher, or 2.2 or higher, or 2.4 or higher, is 2.6 or higher, or 2.8 or higher, or 3.0 or higher, or 3.1 or higher, or 3.2 or higher, This further includes being 3.3 or higher, or 3.4 or higher, and any one of the above A] to I] The composition described. K] Ethylene / α-olefin interpolymer, [(Vinyl / 1000C) / ( The ratio of vinylidene / 1000C is 6.0 or less, or 5.5 or less, or 5.0 or less, is 4.8 or less, or 4.6 or less, or 4.4 or less, or 4.2 or less, or 4.0 or less, or The composition according to any one of A] to J] above, further comprising the fact that is 3.8 or less. L] Ethylene / α-olefin interpolymer is 0.30 or higher, or 0.32 or lower. The above, or 0.34 or more, or 0.36 or more (vinyl / 1000C) amount, further comprising the above A composition described in any one of A] to K]. M] Ethylene / α-olefin interpolymer is 0.60 or less, or 0.58 or less The above further includes an amount of (vinyl / 1000C) less than or equal to 0.56 or less, or 0.54 or less. A composition described in any one of A] to L]. N]ethylene / α-olefin interpolymer is 0.06 or higher, or 0.08 or lower. The above, or further containing 0.10 or more (vinylidene / 1000C), of the above A] to M] The composition described in any one of the following. [O]Ethylene / α-olefin interpolymer is 0.20 or less, or 0.18 or less. The above A] to N] further contain the amount of (vinylidene / 1000C) below or less than 0.16. The composition described in any one of the following: P]ethylene / α-olefin interpolymer, 0.4 2 or more, or 0.44 or more, or 0.46 or more [(vinyl / 1000C) + (vinyllide The composition according to any one of A] to O] above, further comprising the total of n / 1000C). Q] The ethylene / α-olefin interpolymer is 0.61 or less, or 0.60 or less. Below, or 0.59 or less, a combination of [(vinyl / 1000C) + (vinylidene / 1000C)] A composition according to any one of A] to P] above, further comprising the total. R] Ethylene / α-olefin interpolymer, 2.0 g / 10 min or more, or 4 0.0g / 10 minutes or more, or 6.0g / 10 minutes or more, or 8.0g / 10 minutes or more, or 10 0.0g / 10 minutes or more, or 12.0g / 10 minutes or more, or 14.0g / 10 minutes or more, Having a melt index (I2) of 15.0 g / 10 min or higher, any of the above A] to Q] Any one of the compositions described. S] Ethylene / α-olefin interpolymer, 60 g / 10 min or less, or 50 g / 10 min or less, or 45 g / 10 min or less, or 40 g / 10 min or less, or 38 g / 10 Less than 10 minutes, or 36g / 10 minutes or less, or 34g / 10 minutes or less, or 32g / 10 minutes or less A composition according to any one of A] to R] above, having a melt index (I2). T] Ethylene / α-olefin interpolymer is 5.0 or higher, or 5.5 or higher. or 6.0 or higher, or 6.2 or higher, or 6.4 or higher, or 6.6 or higher, or 6.8 or higher, Or having an I10 / I2 of 7.0 or higher, or 7.2 or higher, or 7.4 or higher, or 7.6 or higher. The composition described in any one of the above A] to S]. U] Ethylene / α-olefin interpolymer is 30.0 or less, or 25.0 or less. Below, or 20.0 or less, or 15.0 or less, or 10.0 or less, or 9.0 or less, or 8 I10 values ​​of 0.8 or less, or 8.6 or less, or 8.4 or less, or 8.2 or less, or 8.0 or less A composition according to any one of the above A] to T], having / I2. V] Ethylene / α-olefin interpolymer, 12,000 g / mol or more, or 14,000 g / mol or more, or 16,000 g / mol or more, or 18,000 g / mol or more, or 20,000 g / mol or more, or 22,000 g / mol or more, Or any of the above A] to U] having a number average molecular weight Mn of 24,000 g / mol or more. or one of the compositions described above. W] Ethylene / α-olefin interpolymer, 50,000 g / mol or less, Or 45,000 g / mol or less, or 40,000 g / mol or less, or 38,000 g / mol or less, or 36,000 g / mol or less, or 34,000 g / mol or less, Or, a number-average molecular weight of Mn of 32,000 g / mol or less, or 30,000 g / mol or less. A composition according to any one of the above A] to V], having the following characteristics. X] Ethylene / α-olefin interpolymer, 38,000 g / mol or more, or 40,000 g / mol or more, or 42,000 g / mol or more, or 44,000 g / mol or more, or 46,000 g / mol or more, or 48,000 g / mol or more, Or any of the above A]~W] having a weight-average molecular weight Mn of 50,000 g / mol or more Any one of the compositions described. Y]Ethylene / α-olefin interpolymer, 80,000 g / mol or less, Or 75,000 g / mol or less, or 70,000 g / mol or less, or 68,000 g / mol or less, or 66,000 g / mol or less, or 64,000 g / mol or less, Alternatively, a weight-average molecular weight M of 62,000 g / mol or less, or 60,000 g / mol or less. A composition according to any one of A] to W] above, having n. Z] Ethylene / α-olefin interpolymer is 1.6 or higher, or 1.7 or higher. Alternatively, a molecular weight distribution of 1.8 or higher, or 1.9 or higher, or 2.0 or higher (MWD = Mw / Mn) A composition according to any one of the above A] to Y], having the following characteristics. [AA] Ethylene / α-olefin interpolymer is 2.9 or less, or 2.8 or less. , or 2.7 or less, or 2.6 or less, or 2.5 or less, or 2.4 or less, or 2.3 or less , or having a molecular weight distribution MWD of 2.2 or less, as described in any one of A] to Z] above. composition. Regarding BB] ethylene / α-olefin interpolymer, α-olefin is C 3~C 20 α-olefins, and further C3~C 10 The above A to AA are α-olefins. A composition according to any one of the following: [CC] Ethylene / α-olefin interpolymer And the α-olefin is propylene, 1-butene, 1-pentene, 1-hexene, or 1-Octene, further propylene, 1-butene, or 1-Octene, further 1-butene or 1 -Octene, further selected from 1-octene, as described in one of the above A]~BB]. The composition of. DD] Ethylene / α-olefin interpolymer, ethylene / α-olefin co A polymer, the composition described in any one of the above A] to CC]. [EE] Ethylene / α-olefin interpolymer, below: ethylene / propylene Copolymer, ethylene / butene copolymer, or ethylene / octen copolymer, further E Teylene / butene copolymer, or ethylene / octen copolymer, and further ethylene / octen copolymer A composition according to any one of A] to DD] above, selected from a copolymer. [FF] The composition contains 50.0% or more by weight, or 55.0% by weight, based on the weight of the composition. % or more, or 60.0% by weight or more, or 65.0% by weight or more, or 70.0% by weight or more, or 75.0% by weight or more, or 80.0% by weight or more, or 85.0% by weight or more, or 90 Ethylene / α-O A composition according to any one of A] to EE] above, comprising refyn interpolymer. The composition contains 95.0% or more by weight, or 95.5% by weight, based on the weight of the composition. % or more, or 96.0% by weight or more, or 96.5% by weight or more, or 97.0% by weight or more, Or ethylene at 97.5% by weight or more, or 98.0% by weight or more, or 98.1% by weight or more / A combination of any one of the above A] to FF] containing an α-olefin interpolymer Finished product. The HH composition is 100.0% by weight or less, or 99.8% by weight, based on the weight of the composition. Less than or equal to a certain percentage, less than or equal to 99.6% by weight, less than or equal to 99.4% by weight, or less than or equal to 99.2% by weight, is 99.0% by weight or less, or 98.8% by weight or less, or 98.6% by weight or less, or 98. Ethylene / α-olefin interpolymer in an amount of 4% by weight or less, or 98.3% by weight or less A composition including any one of the above A] to GG]. II) The composition has one or more polymer properties, ethylene / α-olefin in It further contains a second ethylene / α-olefin interpolymer that is different from the terpolymer, Furthermore, one or more polymer properties include comonomer content, I2, I10 / I2, Mn, and Mw. Mz, MWD, or a combination thereof, with one or more polymer properties selected, Mn, Mw, Mz, MWD, or a combination thereof, as selected from the above A]~HH] A composition as described in any one of the following. [JJ] The second ethylene / α-olefin interpolymer is 0.860~0.89 0 g / cc, or 0.865~0.888 g / cc, or 0.865~0.885 g / cc The composition described in [II] above, having a density of c. [KK] The second ethylene / α-olefin interpolymer is 0.5~50g / 10 Melt in minutes, or 1.0-20.0g / 10 minutes, or 5.0-10.0g / 10 minutes A composition according to [II] or [JJ] above, having xx (I2). LL] Regarding the second ethylene / α-olefin interpolymer, α-olefin However, C3~C 20 α-olefins, and further C3~C 10 It is an α-olefin, as described in II above. A composition as described in any one of the following: ~KK] MM] Regarding the second ethylene / α-olefin interpolymer, α-olefin However, propylene, 1-butene, 1-pentene, 1-hexene, or 1-octene, and further pr Lopilene, 1-butene, or 1-octene, further 1-butene or 1-octene, further 1- A composition selected from octen, according to any one of the above [II] to [LL]. [NN] The second ethylene / α-olefin interpolymer is ethylene / α-olefin A composition according to any one of the above [II] to [MM], which is a fin copolymer. OO] The second ethylene / α-olefin interpolymer is: ethylene / pro Pyrene copolymer, ethylene / butene copolymer, or ethylene / octen copolymer, Furthermore, ethylene / butene copolymer, or ethylene / octen copolymer, further ethylene / A composition selected from octen copolymers, according to any one of the above [II] to [NN]. . PP]TGIC Spread Parameter B 1 / 4 However, if it is 7.5 or less, or 7.0 or less, or 6 0.5 or less, or 6.0 or less, or 5.5 or less, or 5.0 or less, or 4.8 or less, or 4 It is 0.6 or less, or 4.4 or less, or 4.2 or less, or 4.0 or less, or 3.8 or less. A composition according to any one of the above A] to OO]. QQ]TGIC Spread Parameter B 1 / 4 However, if it is 1.5 or higher, or 2.0 or higher, or 2 0.2 or higher, or 2.4 or higher, or 2.6 or higher, or 2.8 or higher, or 3.0 or higher, or 3 A composition according to any one of the above A] to OO], wherein the value is 0.2 or higher. [RR] The composition further comprises a peroxide and a silane coupling agent, as described in II above. A composition described in any one of the following: ~QQ. The weight ratio of SS peroxide to silane coupling agent is 0.5 or greater, or 1.0 Above, or 1.5 or above, or 2.0 or above, or 2.5 or above, or 3.0 or above, or 3.5 A composition according to any one of the above A] to RR], wherein the value is 4.0 or higher. The weight ratio of the TT peroxide to the silane coupling agent is 7.0 or less, or 6.5. The above is below, or 6.0 or less, or 5.5 or less, or 5.0 or less, or 4.5 or less. A composition described in any one of A] to SS]. The UU] composition further comprises any of the above A] to TT] (A to TT) Any one of the compositions described. The crosslinking agent is present in an amount of 0.05% by weight or more, or 0.10% by weight, based on the weight of the composition. Amount of % or more, or 0.15% by weight or more, or 0.20% by weight or more, or 0.25% by weight or more , or 0.30% by weight or more, or 0.35% by weight or more, or 0.40% by weight or more, or 0 The composition described above UU, present in an amount of 0.45% by weight or more, or 0.50% by weight or more. . [WW] The crosslinking aid is 3.00% by weight or less, or 2.50% by weight, based on the weight of the composition. Less than % by weight, or 2.00% by weight or less, or 1.50% by weight or less, or 1.00% by weight or less or in an amount of 0.80% by weight or less, or 0.70% by weight or less, or 0.60% by weight or less The composition described above as UU] or VV]. The weight ratio of XX]peroxide to the excipient is 0.5 or greater, or 0.8 or greater, or 1.0 1.5 or more, or 1.1 or more, or 1.2 or more, or 1.3 or more, or 1.4 or more, or 1.5 The above UU]~WW] is either 1.6 or higher, or 1.8 or higher, as indicated in one of the above UU]~WW] The composition of the listed items. The weight ratio of YY peroxide to the excipient is 3.0 or less, or 2.8 or less, or 2.6 The above is below, or 2.4 or less, or 2.3 or less, or 2.2 or less, or 2.0 or less. A composition described in any one of the following: UU]~XX] The weight ratio of the auxiliary agent to the silane coupling agent is 1.0 or greater, or 1.2 or greater, The UU is 1.4 or higher, or 1.6 or higher, or 1.8 or higher, or 2.0 or higher. A composition according to any one of the YY. A3] The weight ratio of the auxiliary agent to the silane coupling agent is 3.6 or less, or 3.4 or less, is 3.2 or less, or 3.0 or less, or 2.8 or less, or 2.6 or less, or 2.4 or less. The composition described in any one of the above UU]~ZZ]. B3] The composition contains 0.05% or more by weight, or 0.10% by weight, based on the weight of the composition. % or more, or 0.15% by weight or more, or 0.20% by weight or more, or 0.25% by weight or more, Or 0.30% by weight or more, or 0.35% by weight or more, or 0.40% by weight or more, or 0. 45% by weight or more, or 0.50% by weight or more, or 0.55% by weight or more, or 0.60% by weight A composition according to any one of A] to A3] above, comprising % or more of peroxide. [C3] Composition is 5.00% by weight or less, or 4.50% by weight, based on the weight of the composition. % or less, or 4.00% by weight or less, or 3.50% by weight or less, or 3.00% by weight or less, Or 2.50% by weight or less, or 2.00% by weight or less, or 1.50% by weight or less, or 1. A composition according to any one of A] to B] above, comprising 00% by weight or less of a peroxide. . [D3] The composition contains 0.05% or more by weight, or 0.10% by weight, based on the weight of the composition. Contains % or more, or 0.15% or more by weight, or 0.20% or more by weight of a silane coupling agent. The composition described in any one of the above A] to C3]. E3] The composition is 3.00% by weight or less, or 2.50% by weight, based on the weight of the composition. % or less, or 2.00% by weight or less, or 1.50% by weight or less, or 1.00% by weight or less, Alternatively, the above includes a silane coupling agent in an amount of 0.80% by weight or less, or 0.60% by weight or less. A composition described in any one of A] to D3]. F3] The composition contains 99.0% or more by weight, or 99.1% by weight, based on the weight of the composition. Interpolymers, peroxides, or The total of oxides and silane coupling agents, as described in any one of the above A] to E3] The composition of the listed items. G3] The composition is 100.0% by weight or less, or 99.9% by weight, based on the weight of the composition. Less than or equal to a certain percentage, less than or equal to 99.8% by weight, less than or equal to 99.7% by weight, or less than or equal to 99.6% by weight, It contains 99.5% by weight or less of interpolymers, peroxides, and silane coupling agents. A composition according to any one of the above A] to F3], including the total. The H3 composition is selected from UV stabilizers, antioxidants, or combinations thereof. A composition according to any one of A] to G3] above, further comprising at least one additive. I3] At least one additive is present in an amount of 0.01% by weight or more, based on the weight of the composition. or 0.02% by weight or more, or 0.03% by weight, or 0.04% by weight or more, or 0.06 The above H is present in an amount of % by weight or more, or 0.08% by weight or more, or 0.10% by weight or more. The composition described in [3]. J3] At least one additive is present in an amount of 2.00% by weight or less of the composition, Or 1.50% by weight or less, or 1.00% by weight or less, or 0.80% by weight or less, or 0. Present in amounts of 60% by weight or less, or 0.40% by weight or less, or 0.20% by weight or less, The composition described in [H3] or [I3]. K3] A crosslinked composition formed from any one of the compositions described in A] to J3] above. . [L3] The composition has a value of 5.00 or higher, or 5.10 or higher, or 5.15 or higher, or 5.2 MH values ​​of 0 to 5.22, or 5.24 or 5.26 or 5.28 or higher A composition according to any one of the above K3] having a value of -ML. The M3 composition has a gel content of 84% or more, or 85% or more, or 86% or more (4+ The composition according to K3] or L3] above, having 12 minutes. N3] At least one composition formed from any one of the compositions described in A] to M3] above An article containing one component. O3] Articles include film, further extruded film and / or cast film, further extruded The item described in [N3] is a film. The article described in [N3], wherein the article in [P3] is a solar cell module. Q3] A process for forming a solar cell module, wherein the process comprises two steps This includes stacking an array of solar cells between film layers, with each film layer independently being the above A process formed from any one of the compositions described in A] to M3]. R3] The process according to Q3] above, wherein each film layer is formed from the same composition. S3] Solution polymerization process for preparing ethylene / α-olefin / interpolymer The process involves ethylene in a single reactor at a reactor temperature of 150°C or higher. A reaction mixture comprising len, α-olefin, solvent, and a metal complex selected from a) below. A solution polymerization process, which includes polymerizing a material. a) Select from the following structures 1 as described above in the Outline of Invention (SOI). Biphenylphenol metal complex: [ka] T3] For structure 1, L is -(CH2)n- (where n=2~4), -C H2C(R a R b )CH2-(wherein, R a and R b These are independent of each other, (C1~C4 0) Hydrocarbyl, (C1~C 40 )heterohydrocarbyl, or -H), or -CH2Ge(R D )2CH2- or -CH2Si(R D )2CH2-(in the formula, each R D These are independently -H, C 1 (~C40) Hydrocarbyl, (C1~C 40 ) Heterohydro Calville, -Si(R C )3, -Ge(R C )3, -P(R P )2, -N(R N )2, - Ure C , -SR C -NO2, -CN, -CF3, R C S(O)-, R C S(O)2- (R C )2C=N-, R C C(O)O-, R C OC(O)-, R C C(O)N(RN )- , and (R N ) Selected from the group consisting of 2NC(O)-, and In Structure 1, each R C , R P , and R N However, independently, (C1~C 30 ) Hydrocal Building, (C1~C 30 ) Heterohydrocarbyl, or -H, as described in S3 above Rothes. U3] Regarding structure 1, -Z 1 - and -Z 2 -Each of these is -O-, as in S3 above] Or the process described in T3. V3] For structure 1, R 1 or R 8 at least One is selected from radicals having formula (II) or radicals having formula (I), The process described in one of the following [S3]~U3]. W3] Regarding Structure 1, R 1 and R 8 These are identical and have the radical (I), A selection is made from the group consisting of radicals having formula (II) and radicals having formula (III). The process described in any one of the above S3 to V3. X3] Regarding structure 1, R 1 =R 8 = The radical having formula (II), above S3 The process described in one of the following: ]~W3]. Regarding equation (II) of structure 1 in Y3, R 43 =R 46 = non-substituted alkyl, further non-substituted (C1~C 10 )alkyl, further unsubstituted (C1~C8)alkyl, further unsubstituted (C1~C 6) Alkyl, further unsubstituted (C1-C4) alkyl, and further t-butyl, as described above for X3] The process described above. Regarding equation (II) in Z3, 41 =R 42 =R 44 =R 45 =R 47 =R 48 =H The process described in X3] or Y3] above. A4] Regarding structure 1, L is -CH2C(R a R b )CH2-(wherein, R a and R b Each of them is independent, (C1~C 40 ) Hydrocarbyl, (C1~C 40 ) Heterohy Drocarbil, or -H), or -CH2Ge(R D )2CH2-, or -C H2Si(R D )2CH2-(in the formula, each R D These are independently -H, (C1~C 40 ) Hidden Locarvir, and (C1~C 40 (Selected from heterohydrocarbyl) A process described in any one of the above S3 to Z3. B4] Regarding structure 1, L is as follows: i)-CH2Si(R a )(R b )CH2- or -CH2Ge(R a )(R b )C H2-(wherein, R a and R b Each of them is independent, (C1~C 30 ) Hydrocarbyl or (C1~C 30 (It is a heterohydrocarbyl.) ii) 1,3-dimethylpropane-1,3-diyl, iii) Bis(methylene)cyclohexane-1,2-diyl, iv) Propane-1,3-diyl, or iv) One of the above S3]~A4] selected from butane-1,4-diyl The process described below. Regarding structure 1 in C4, L is as follows: i)-CH2Si(R a )(R b )CH2-(wherein, R a and R b These are each German Standing, non-substitution (C1~C 10 )alkyl, further unsubstituted (C1~C8)alkyl, further non Substituted (C1-C6) alkyl, further unsubstituted (C1-C4) alkyl, further unsubstituted (C1- C3) alkyl) ii) 1,3-dimethylpropane-1,3-diyl, or iii) Selected from bis(methylene)cyclohexane-1,2-diyl, as described above. The process described in one of the following: S3 to B4. For structure 1 of D4, n=2, and each X is the same and is an unsubstituted alkyl group. or any one of the processes described in S3 to C4 above. E4] Each X is an unsubstituted (C1-C3) alkyl, and further unsubstituted (C1-C2) alkyl Furthermore, the process described in D4 above, which is methyl. F4] For structure 1, R10 = R15, one of the above S3] to E4] The process described above. Regarding structure 1 in G4, R10 = R15 = halogen, and furthermore, F, as in S3 above, ~F The process described in any one of [4]. H4] For Structure 1, R3 = R6, as described in one of the above S3] to G4]. The loading process. Regarding structure 1, R3=R6=unsubstituted alkyl, as described above for S3]~H4] The process described in any one of the following. J4] For structure 1, R3 = R6 = non-substituted (C1~C 12 ) alkyl, and further unsubstituted (C1~C 10) alkyl, further unsubstituted (C2~C8) alkyl, further unsubstituted (C4~C 8) Alkyl, and furthermore, unsubstituted C8 alkyl, as described in any one of the above S3] to I4] The loading process. K4] For structure 1, R2=R4=R5=R7=R9=R11=R12=R13= The process described in any one of the above S3 to J4, where R14=R16=H. Regarding structure 1 in L4, the metal M = Zr, and one of the above S3 to K4... The process described. The M4 structural formula is selected from the following structures (1a) or (1b). The process described in any one of the following sections: [S3]~L4] [ka] N4] The process described in M4] above, wherein structure 1 is structure (1a). The O4 reaction mixture contains co-catalyst-1 containing borate and co-catalyst-2 containing almoxane. The process described in S3 to N4, which further includes the above. [P4] If the process is above 155°C, or above 160°C, or above 165°C, or 17 0°C or above, or 175°C or above, or 180°C or above, or 185°C or above, or 186°C or above , or reactor temperature of 187°C, or 188°C or higher, or 189°C or higher, or 190°C or higher So, 2.5 × 10 6 The above, or 2.6 × 10 6 The above, or 2.8 × 10 6 The above, or 3. 0 x 10 6 The above, or 3.2 × 10 6 The above, or 3.4 × 10 6 The above, or 3.6 × 10 6 The above, or 3.7 × 10 6 The above, or 3.8 × 10 6 The above, or 3.9 × 10 6 That's all. or 4.0 × 106 The above, or 4.1 × 10 6 The above, or 4.2 × 10 6 The above is an overall The above, having a catalytic efficiency [(grams of interpolymer) per (grams of total catalytic metal)] The process described in S3 to O4. Q4] The process is 0.860~0.900 g / cc, or 0.865~0.890 g / cc, or 0.868-0.880 g / cc of ethylene / α-olefin / international Polymer density: 2.5 × 10 6 The above, or 2.6 × 10 6 The above, or 2.8 × 10 6 Below Top, or 3.0 × 10 6 The above, or 3.2 × 10 6 The above, or 3.4 × 10 6 The above, or 3.6 × 10 6 The above, or 3.7 × 10 6 The above, or 3.8 × 10 6 Above, or 3.9× 10 6 Above, or 4.0 × 10 6 The above, or 4.1 × 10 6 The above, or 4.2 × 10 6 Below The overall catalytic efficiency above [(grams of interpolymer) per (grams of total catalytic metal)] The process described in S3 to P4 above. R4] If the process is above 155°C, or above 160°C, or above 165°C, or 17 0°C or above, or 175°C or above, or 180°C or above, or 185°C or above, or 186°C or above , or reactor temperature of 187°C, or 188°C or higher, or 189°C or higher, or 190°C or higher The processes described above in S3]~Q4] are executed on [the specified machine]. S4] The process is below 250°C, or below 240°C, or below 230°C, or 22 The above S3 is carried out at a reactor temperature of 0°C or below, or 210°C or below, or 200°C or below. The process described in any one of the following ~R4]. T4] The reactor is a continuous stirred-tank reactor, a loop reactor, or a plug-flow reactor (or tubular type) A reactor, further selected from a continuous stirred tank reactor or a loop reactor, and further selected from a continuous stirred tank reactor. The process described in any one of the above S3 to S4. U4] The reaction mixture further contains hydrogen (H2), one of the above S3] to T4] The process described above. V4] Ethyl formed by any one of the processes described in S3] to U4] above A composition containing a len / α-olefin interpolymer. W4] TGIC spreading pack of polymer composition containing one or more olefin polymers Lameta B 1 / x A method for determining such a method as described in SOI A method that includes steps. X4] The composition contains 50% or more by weight, or 60% or more by weight, based on the weight of the composition. or 70% by weight or 80% by weight or 85% by weight or 90% by weight or or 92% or more by weight, or 94% or more by weight, or 96% or more by weight, or 98% or more by weight, or the method described in W4] above, comprising 99% by weight or more of one or more olefin polymers. . [Y4] The composition is 100% by weight or less, or 99% by weight or less, based on the weight of the composition. or containing one or more olefin polymers in an amount of 98% by weight or less, or 95% by weight or less, The method described in [W4] or [x4] above. The composition in Z4 contains only one olefin polymer, as described above in W4 to Y4. Either one of the methods. A5] Ethylene-based polymers, ethylene / α-olefin interpolymers, and further ethylene The method according to any one of the above Z4], wherein the polymer is a ethylene / α-olefin copolymer. B5] The support material is 10% or more by weight, or 20% or more by weight, based on the weight of the support material. Above, or 30% or more by weight, or 40% or more by weight, or 50% or more by weight, or 60% or more by weight Above, or 70% or more by weight, or 80% or more by weight, or 85% or more by weight, or 90% or more by weight Above, or 92% or more by weight, or 94% or more by weight, or 96% or more by weight, or 98% or more by weight The above, or containing 99% or more by weight of graphite, as described in one of the above W4] to A5] Method of loading. C5] The support material is 100% or less by weight, or 99% by weight, based on the weight of the support material. Graphite of the above, or 98% or more by weight, or 95% or more by weight, or 90% or more by weight Including the method described in any one of the above W4 to B5. Regarding step d) of the method in D5), the temperature is from 25°C to 170°C, and further from 30°C to 165℃, and then further increasing from 30℃ to 160℃, as indicated in one of the above W4]~C5] Method of loading. E5] HDPE is M 2.3~3.0, or 2.4~2.9, or 2.5~2.8 WD, and 100,000-140,000 g / mol, or 105,000-135, 000 g / mol, or 110,000~130,000 g / mol, or 115,000 It has a weight-average molecular weight reported in polyethylene equivalents ranging from 0 to 125,000 g / mol. or the method described in any one of the above W4 to D5. F5]B 1 / x Regarding the values, x = 1.5 to 6, then x = 2 to 6, then x = 3 to 6, and so on. The method described in any one of the above W4 to E5, where x = 4 to 6. G5) The support material further comprises a filler as described in any one of W4] to F5] above. method.

[0066] Test method MDR trial The curing properties are determined by Alpha Technologies' Moving Die Rh Using the eometer (MDR)2000 E, according to ASTM D5289, 0 Measurements were taken in a 0.5-degree arc. For each composition, approximately 4 g of pellets were packed into the MDR. R was run at 150°C for 30 minutes, and a "time vs. torque" profile was created at a given interval. The following data was used for each MDR run: MH(dNm), i.e., between 30-minute trials. The maximum torque exerted by the MDR during the interval (this is typically exerted at the 30-minute mark) Corresponding to torque; ML (dNm), i.e., by MDR during a 30-minute test interval. The minimum torque applied (this usually corresponds to the torque applied at the start of the test interval) ; and T90 (the time required to reach 90% of the MH value).

[0067] Gel content test Each cured film prepared from the lamination process (see Experiment section) is "3mm x 3mm The sample was cut into small pieces (approximately 0.5g, Ws). Then, the sample was packed into a metal mesh (Me The sachet number is 120 (weight of Wt1), soak this in 100 ml of xylene at room temperature for 24 hours. It was placed in a 250 ml glass bottle containing [the substance]. Then, the metal mesh and the sample were placed in a condenser. It was then transferred to a 500 ml flask containing 350 ml of xylene. While stirring... Then, after refluxing in boiling xylene for 5 hours, the packed sample was removed from the xylene and vacuum was applied. The sample was placed in an oven and heated under vacuum at 120°C for 2 hours until it reached a certain weight. Finally, the sample was weighed together with a metal mesh of weight Wt2. The gel content was expressed using the equation: gel Content=[(Wt2-Wt1) / Ws] * Calculated by 100%. Xylylene used The compound has a purity of 99% or more, and contains a mixture of ortho, meta, and para isomers, and ethyl This is an AR grade product that may contain benzene.

[0068] Gel permeation chromatography The chromatography system is equipped with an internal IR5 infrared detector (IR5) and Po High-temperature GPC chromatography at lymerChar GPC-IR (Valencia, Spain) It was composed of F. Set the autosampler oven compartment to 160 degrees Celsius, The RAM compartment was set to 150 degrees Celsius. The column has four AGILENT "M The chromatograph used was a 30cm, 20-micron linear mixed-bed column called "ixed A". The solvent contains 200 ppm butylated hydroxytoluene (BHT) 1,2 The solvent source was 4-trichlorobenzene. The solvent source was spurged with nitrogen. The injection volume used was The volume was 200 microliters, and the flow rate was 1.0 milliliter / minute.

[0069] Calibration of GPC column sets with molecular weights in the range of 580 to 8,400,000 The experiment was conducted using 21 polystyrene standards with narrow molecular weight distributions, and there were small differences between the individual molecular weights. The standard substance was placed in six "cocktail" mixtures that were spaced at least 10 times apart. Purchased from Gilent Technologies. Contains over 1,000,000 molecules. Regarding the quantity, it is "0.025 grams in 50 milliliters of solvent," which is 1,000,000. For molecular weights less than a certain amount, the measurement is given as "0.05 grams in 50 milliliters of solvent" for polystyrene. A standard substance was prepared. The polystyrene standard substance was gently stirred at 80 degrees Celsius for 30 minutes. It dissolved while... The peak molecular weight of the polystyrene standard substance was determined using formula 1, and polyethylene... Converted to molecular weight (Williams and Ward, J. Polym. Sci., As described in Polym. Let., 6, 621 (1968):

number

[0070] A quintic polynomial was used to fit the equivalent calibration point for each polyethylene. By making slight adjustments (approximately 0.375 to 0.445), the column resolution and band expansion effect are improved. This is corrected so that a linear homopolymer polyethylene standard material can be obtained at 120,000 Mw. did.

[0071] The total plate count of the GPC column set is calculated by decanning (50 ml TCB) The procedure was performed using a solution prepared with 0.04 g of the medium-sized solution, which was dissolved for 20 minutes while gently stirring. Plate count (Equation 2) and symmetry (Equation 3) are calculated by injecting 200 microliters as follows: The formula:

number

number

[0072] The sample was processed using PolymerChar's "Instrument Control" software. The sample was prepared using a semi-automatic method with a WARE, and then weight-targeted at 2 mg / ml using Polym via a high-temperature autosampler, a scepter cap equipped with pre-spurged nitrogen is used. A solvent (containing 200 ppm BHT) was added to the ial. The sample was subjected to "low-speed" shaking. Then, it was dissolved at 160 degrees Celsius for 2 hours.

[0073] Mn (GPC) , Mw (GPC) , and Mz (GPC) The calculation is performed by PolymerC har GPCOne® software, at each equally spaced data retrieval point (i) IR chromatogram with the slanted line subtracted, and the narrow standard calibration curve of point (i) from Equation 1. Using the polyethylene equivalent molecular weight obtained from, PolymerCha according to Equations 4-6 Using the internal IR5 detector (measurement channel) of a GPC-IR chromatograph, Based on PC results, equations 4-6 are as follows:

number

[0074] To monitor deviations over time, the PolymerChar GPC-IR system A flow marker (decane) was introduced into each sample via a controlled micropump. Flow rate markers (FM) are used to determine the respective decane peaks (RV) within the sample. FM samples)) are compared to decane peaks within a narrow standard calibration (RV (FM calibrated)) and RV By matching the values, the pump flow rate (apparent flow rate) of each sample is linearly corrected. It was used for this purpose. Then, any time change of the Decane marker peak is used for the total flow rate (flow). It was estimated to be related to a linear shift in the quantity (effective).

[0075] To facilitate the highest accuracy in RV measurement of flow marker peaks, least squares fitting is used. Using a chromosome, the peaks in the flow marker concentration chromatogram were fitted to a quadratic equation. Next, the true peak position was determined using the first derivative of the quadratic equation. (Flow marker) After calibrating the system based on the peak, the effective flow rate (with respect to the narrow standard calibration) is given by Equation 7. The calculation was as follows: Effective flow rate = Apparent flow rate * (RV (FM calibrated) / RV (FM Sample (EQ7).

[0076] Processing of flow marker peaks using PolymerChar GPCOne™ software. This was done via software. The allowable flow correction is when the effective flow rate is + / - 0 of the apparent flow rate. Keep it within 7%.

[0077] 1H NMR method Sample preparation. Place the sample in a NORELL 1001-7, 10 mm, NMR tube. Approximately 130 mg of the sample was mixed with 3.25 g of "0.001 M Cr(AcAc)3 containing 50 By adding it to 50 wt tetrachloroethane-d2 / perchloroethylene Prepared. To prevent oxidation, N2 was added as a solvent via a pipette inserted into the tube. The sample was purged by bubbling for approximately 5 minutes. Next, the tube was capped. The sample was then sealed with TEFLON tape and immersed overnight at room temperature to promote its dissolution. During storage and before and after preparation, the sample is kept in an N2 purge box to minimize exposure to O2. The sample was held in place. The sample was heated to 115°C and vortexed to ensure homogeneity.

[0078] Data acquisition parameters and data analysis. 1 1H NMR was performed using a Bruker high-temperature cryogenic system. A Bruker AVANCE 600MHz spectrometer equipped with a probe was used at 120°C. The procedure was performed at the sample temperature. Spectra for quantifying total polymer protons, control spectrum. Two experiments were performed to obtain the signal, suppressing the strong peaks associated with polymer chains and terminal groups. Perform a dual presaturation experiment to enable highly sensitive spectra for quantification. The control was performed using a ZG pulse, 4 scans, SWH 10,000Hz, AQ 1.82s. The experiment was performed in D114s. A dual presaturation experiment was conducted using a modified pulse sequence. S, lc1prf2.zz, TD32768, 64 scans, DS2, SWH9,000 Hz, AQ1.82s, D12s, D 13 The procedure was performed using 12s. The unsaturation measurement was performed as follows: The method described was followed. The resonance area from the polymer chain (i.e., within the polymer) The CH, CH2, and CH3 of the above were obtained during the first experiment (control spectrum) described above. The measurements were taken from the obtained spectra. Four major unsaturated areas (i.e., vinyl, vinyl Len, trisubstituted, and vinylidene) as the second (presaturation) substance described above. The measurements were taken from the spectra obtained during the experiment. Both spectra were taken from the resonance area from the solvent. In contrast, it was normalized. The moles of each unsaturated component, the area under unsaturated resonance, and the components contributing to that resonance were... The calculation was performed by dividing by the number of protons in the polymer. Divide the area below the peak (i.e., CH, CH2, and CH3 in the polymer) by 2. This was calculated by the following: Next, the amount of total unsaturation was calculated by the moles of total unsaturation and the amount of carbon in the polymer. It is expressed as a relative ratio to 'L' and represented by the number of unsaturated atoms per 1000 carbon atoms.

[0079] Melt Index The melt index (I2) of ethylene polymers is defined in ASTM D-1238. The measurement is performed according to 190℃ / 2.16kg (melt index (I10) is 19 (0℃ / 10.0kg). I10 / I2 was calculated from the ratio of I10 to I2. Propylene The melt flow rate (MFR) of the polymer system is based on ASTM D-1238, under conditions of 230°C. Measured according to / 2.16kg.

[0080] Polymer density Polymer density is measured according to ASTM D-792.

[0081] High-temperature thermal gradient interaction chromatography (HT-TGIC, or TGIC)-TGI Determination of the C-spread parameter Commercially available crystallization elution fraction analyzer Using CEF (Polymer Char, Spain), TGIC measurements were performed. (Cong, et al., Macromolecules, 2011, 44(8), 3062-3072). The CEF instrument is equipped with an IR-5 detector. Graphite , used as the stationary phase in the HT-TGIC column (Freddy, A. Van Dam) me et al., US8,476,076, Winniford et al., U S8,318,896.). Separation using a single graphite column (250 × 4.6 mm). It was used for the following: Graphite, dry filling technique, followed by dry filling, followed by wet filling technique. The column was packed using (Cong et al., EP2714226B1 and References used). Graphite (substantially non-porous with high crystallinity), Sup Obtained from error Graphite. The experimental parameters were as follows: Oven / Transfer line / Needle temperature 150°C, Dissolution temperature 150°C, Dissolution stirring setting 2, Pump Stabilization time 15 seconds, pump flow rate for column washing 0.500 mL / m, column packing Pump flow rate 0.300 ml / min, stabilization temperature 150°C, stabilization time (pre-packing of column, (Before packing) 2.0 min, Stabilization time (post-packing of column, after packing) 1.0 min, SF (soluble) (Periodic fraction) Time 5.0 minutes, Cooling rate from 150°C to 30°C 3.00°C / min, Cooling process Flow rate of 0.04 ml / min, heating rate from 30°C to 160°C of 2.00°C / min, at isothermal temperature Intermittent injection at 160°C for 10 minutes, with an elution flow rate of 0.500 mL / min and an injection loop size of 200 mm. Chlorite. Flow rate during the cooling process, all polymer fractions, at the end of the cooling cycle. The length of the graphite column was adjusted so that the material would remain on the column.

[0082] The sample was prepared using a PolymerChar autosampler at 150°C for 120 minutes, OD Prepared at a concentration of 4.0 mg / ml in CB (defined below). Silica gel 40 (particle size 0. 2-0.5mm, catalog number 10181-3, EMD) in a vacuum oven at 160℃ It was dried. In the case of a CEF instrument equipped with an autosampler with N2 purging capability, Ricagel 40 was placed in three 300 x 7.5 mm GPC-sized stainless steel columns. Fill the silica gel 40 column and attach it to the pump inlet of the CEF instrument, then use the ODCB. Dry it. This "ODCB dried with silica gel" will be referred to as "ODCB" here. .

[0083] TGIC data is used by PolymerChar (Spain)'s "GPC One" software. Processed on a tower platform. Temperature calibration was performed using approximately 2-6 mg of EICOSANE. 14.0 mg isotactic homopolymer polypropylene iPP (150,000~ The molecular weight Mw, reported as the polyethylene equivalent of 190,000 g / mol, is 3.6-4. The polydispersity of 0 (Mw / Mn), where the DSC dissolution temperature of iPP is 158-159°C. The procedure was carried out with a mixture of (DSC method as described herein below) that was measured to be present. 14 0.0 mg linear homopolymer polyethylene HDPE (comonomer content zero, 115, Weight-average molecular weight reported as polyethylene equivalent in the range of 000 to 125,000 g / mol ( Mw), and polydispersity of 2.5-2.8, are used in a 7.0 mL ODCB filled with "10m It was added to an "L vial". The dissolution time was 2 hours at 160°C.

[0084] For the calibration process, solutions of EICOSANE, iPP, and HDPE were used. For elution temperatures in the range of 30°C to 150°C, the process consists of the following steps. 1. Extrapolate the elution temperature of each isothermal step during elution according to the heating rate (see Figure 1). (As shown). The solid line is experimental data. The dashed line is the extrapolation of the elution temperature for two isothermal steps. be. 2. Calculate the delay amount. The maximum value of the EICOSANE peak (y-axis) is the value of the solution at 30.0°C. To match the output temperature, the temperature corresponding to the IR measurement channel chromatogram (y axis) ( The x-axis is shifted. The delay amount is the actual temperature difference (30℃ - EICOSANE peak maximum value). The elution temperature is calculated by dividing it by the heating rate of the method and then multiplying it by the elution flow rate. 3. Adjust each recorded elution temperature using the same delay adjustment. 4. The observed HDPE reference had a peak elution temperature of 150.0°C, while E The heating rate was linearly controlled so that the ICOSANE elution peak temperature was maintained at 30.0°C. Scaling to TGIC chromatography of EICOSANE / iPP / HDPE mixture. The ram is shown in Figure 2.

[0085] At least 20 ethylene octene random copolymers are used with a single-site catalyst. It is produced using a method with a Mw (ethylene equivalent weight-average molecule) in the range of 36,000 to 150,000. Each ethylene octene copolymer has a quantity and a polydispersity (MWD) of 2.0 to 2.2. The measured elution peak temperature (Tp) and the octene content (wt%) of the copolymer are shown in Figure The correlation specified in 3 is followed. The molecular weight distribution is measured according to the reference (Cong et al.). al., Macromolecule, 2011, 44(8), 3062-3072). The octene content is determined according to (Li et al., US7,608,668 and cited references). It is then measured by 13C NMR.

[0086] Data processing for HT-TGIC polymer samples A solvent blank (injected with high-purity solvent) was performed under the same experimental conditions as the polymer sample. - For sample data processing, the following: subtraction of solvent blanks in each detector channel, comparison Temperature extrapolation as described in the positive process, and using the delay amount determined from the calibration process. Dissolution temperature axis in the range of 30°C to 160°C, calculated from the temperature compensation and calibration heating rate. Adjustments can be made.

[0087] Chromatogram (measurement channel of IR-5 detector) PolymerChar Integrated with GPC One software. Peaks are flat at high elution temperatures. (Approximately zero value in blank subtraction chromatogram), and soluble fraction If the detector signal on the high-temperature side (on, SF) falls to the minimum or flat region, is it a visible difference? Then I drew a straight baseline.

[0088] The melting point of homopolymer polypropylene specified by the HT-TGIC melting point of iPP is indicated It is determined using a differential scanning calorimeter (DSC). The temperature at the maximum heat flow rate relative to the linear baseline was used as the melting point. The structure is constructed from the start of melting (above the glass transition temperature) to the end of melting. The temperature is The temperature is raised from room temperature to 200°C at a rate of 10°C / min, maintained at 200°C for 5 minutes, and then reduced to 0°C at a rate of 10°C / min. The temperature is lowered by 10°C / min, maintained at 0°C for 5 minutes, and then the temperature is increased from 0°C to 200°C in increments of 10°C / min. The temperature is raised for several minutes, and data is obtained from this second heating cycle.

[0089] TGIC profile spread parameter, B 1 / x Calculation Here, parameter B 1 / x The common ingredients in both the comparative sample and the sample of the present invention —The respiration of the distribution was defined from TGIC measurements to quantify it (see, for example, Figure 4). The following procedure is used to obtain B from TGIC measurements. 1 / x This section describes how to calculate it. 1. In accordance with the TGIC method described above, the test sample and EICOSANE / iPP / HDPE Run both parts of the mixture in the same run queue. 2. Generate a TGIC chromatogram (dwi / dT vs. elution temperature (T) profile). do. 3. For the test samples, each data point with the highest intensity between 35.0°C and 170.0°C was investigated. By doing so, the maximum height is taken from the TGIC chromatogram (dwi / dTi vs. temperature). The corresponding elution temperature of the TGIC chromatogram at the maximum height is obtained as the profile temperature. Defined as Tp). The TGIC chromatogram has multiple peaks (excluding SF peaks). If it is present and multiple peaks have exactly the same peak height, then the peak at the highest dissolution temperature This is defined as the profile temperature (Tp). The profile width (maximum height at 1 / x) is also defined. ) is defined as the temperature difference between the front temperature and the rear temperature at 1 / x of the maximum height. The forward temperature at 1 / x of height was investigated from 35.0°C forward, and the backward temperature at 1 / x of maximum height. The temperature is investigated in reverse order, starting from 170.0°C. 4. HDPE peak height from EICOSANE / iPP / HDPE reference (1 / x) Calculation of the peak width of HDPE at 1 / x of the peak width (at a elution temperature of 150.0°C) (Figure 2) (See reference). 5. Next, based on the following formula, B 1 / x The following is calculated:

number

[0090] TGIC spread parameter (for example, B 1 / 4 ) is ethylene / α-olefin in This is an indicator of the respiration of the comonomer distribution in terpolymers. Smaller B 1 / 4 The value is narrower Shows the comonomer distribution. Narrow comonomer distribution (smaller B 1 / x ) contains PV encapsulant It was found to be advantageous for the curing effect of POE in TGIC chromatography. This is an important technique for determining the characteristics of comonomer content and its distribution (see Figure 3). ). A specific percentage of the height of the maximum (mass intensity) peak in the TGIC profile. The respiration of the comonomer distribution can be quantified using the peak width (°C). However, the peak width The absolute value of is also related to chromatography-related experimental factors (Stregel, et al.). ,“Modern size-exclusion liquid chromatog raphy, Wiley, 2 nd edition, Chapter 3) and / or tree It may be affected by the lipid comonomer content. In this case, the distribution of comonomers To minimize bias from experimental factors and comonomer content in polymers B 1 / x Defined by using parameters.

[0091] experiment Commercial polymers and additives Ethylene / 1-octene random copolymer: Density 0.873 g / cc, I2 14 g / 10 min (XUS 38669, manufactured by The Dow Chemical Company) Polyolefin elastomer). This copolymer is referred to as "POE 669" in the table below. It will be listed as ".

[0092] ENGAGE 8407 Polyethylene by The Dow Chemical Company Olefin elastomer, ethylene / 1-octene random copolymer: density 0.870 g / cc, I2 30g / 10 min, listed as POE 407 in the table below.

[0093] TBEC: tert-butylperoxy-2-ethylhexyl carbonate, Ark EMA-manufactured LUPEROX TBEC organic peroxide. VMMS:3-(trimethoxysulfate Lylpropyl methacrylate, a silane coupling agent manufactured by Dow Corning. Bridge auxiliaries: Triaryl isocyanurate (TAIC).

[0094] Polymer synthesis and properties The interpolymer is subjected to a 1-gallon polymerization reaction, which is filled with hydraulic pressure and operated under steady-state conditions. Each was prepared in a receiving vessel. The catalyst and co-catalyst are listed in Table 1. Solvent, hydrogen, catalyst, and The co-catalyst was supplied to the reactor according to the process conditions outlined in Tables 2A-2C. The solvent was: ISOP supplied by ExxonMobil Chemical Company The result was AR E. The reactor temperature was measured at or near the reactor outlet. Interpoli The mar was isolated and pelletized.

[0095] The POE characteristics are summarized in Table 3. The unsaturation measurements from 1H NMR are summarized in Table 4. The GIC results are summarized in Table 5.

[0096] [Table 1]

[0097] [Table 2]

[0098] [Table 3]

[0099] [Table 4]

[0100] [Table 5]

[0101] [Table 6]

[0102] [Table 7]

[0103] POE peroxide curing compound Tables 6 and 7 show the POE peroxide cured compositions. Peroxide, auxiliary agent, and silamine. To enable thorough mixing of the polymer pellets into the formulation, polymer pellets (98.25g) are used. Amount %) is used as a curing additive (1.00 wt% peroxide, 0.50 wt% crosslinking aid, and Along with 0.25% by weight of a silane coupling agent, a encapsulable fluorinated high-density polyethylene It was immersed in a glass bottle. After 5 hours at 50°C, no liquid residue was visible on the bottle. The immersion (absorption) process was carried out until the peroxide, silane, and auxiliary agents were absorbed into the pellet. Therefore, to ensure homogeneous absorption, the bottle is opened every 30 minutes during the absorption process. It was shaken for 0 seconds.

[0104] Layered sample preparation Using two slightly different preparation conditions (A and B below), crosslinked POE film The following were prepared. A PENERGY L036 laminator was used for each preparation.

[0105] A) Sample preparation by a lamination process using a glass substrate (Table 6). In the laminator, approximately 2.5g of pellets absorbed peroxide, silane, and auxiliary agents. The "sample" is placed on a PTFE film (0.24 mm thick) and a glass substrate (3 mm thick). A metal frame with a thickness of 1 mm was placed on the top surface. A metal frame was used as a spacer around the sample. It was then placed in a different PTF and confirmed that the cross-linked POE had a thickness of approximately 1 mm. A 0.24 mm thick E film was placed on the top surface of the sample. Lamination was performed at a set temperature of 150°C. It was done at a certain temperature. The heating process consisted of the following two steps: Step 1: Vacuum (- Preheat at 100kPa for 4 minutes without pressure, then step 2: pressurize at 1 bar for 12 minutes. These are some examples. After the lamination cycle, the cross-linked film was removed for further gel measurement.

[0106] B) Sample preparation by a lamination process using a metal substrate (Table 7). In the laminator, approximately 2.5g of pellets absorbed peroxide, silane, and auxiliary agents. The "sample" is placed on a PTFE film (0.24 mm thick) and a metal substrate (1.8 mm thick). It was placed on the top surface. A PTFE frame with a thickness of "0.5 mm" was used as a spacer. We placed it around the sample and confirmed that the cross-linked POE had a thickness of approximately 0.5 mm. Next... Then, another PTFE film (0.24 mm thick) was placed on the top surface of the sample. The lamination was 1 The process was carried out at a set temperature of 50°C. The heating process consisted of the following two steps: Step 1: Preheat under vacuum (-100kPa) without pressure for 4 minutes. Step 2: 1 bar Pressurization is performed for 10 or 16 minutes. After the lamination cycle, crosslinking is performed for further gel measurement. I took out the film.

[0107] Measurement of adhesion to glass after lamination The film (100mm x 150mm x 0.5mm) was preheated for 4 minutes under the following conditions: Using no pressure, 100°C, 100 MPa, and 100°C for 2 minutes, Lab Tech L The product was prepared by compression molding of the compounded resin pellets using a PS-50 compression molding machine. After shaping, the film is placed on a glass substrate (dimensions 100mm x 150mm x 3mm). Next, it was covered with a polyester backsheet. Then, under the following conditions: vacuum (-100kP) a) Preheat the sample for 4 minutes without pressure, then use a pressure of 1 bar for 16 minutes, and then use the 150 bar pressure setting. The material was subjected to a lamination process at °C (using a SHUNHONG SH-X-1000 laminator).

[0108] After lamination, the laminated film and backsheet are further cut into "1 inch width" and "1 inch width" respectively. It was divided into three strips, each 50 mm long. Using an INSTRON 5565, For the three test specimens, peel off the laminated film and backsheet from the glass substrate. A "180° peel test" was conducted. The average of the three results is reported.

[0109] Summary of results Regarding the manufacturing process of PV encapsulant film, the processability of the compounded materials is determined by the extrusion process. Constrained by shear heating of polymers in ces. Per in PV encapsulant film formulations The oxide decomposes at temperatures above 110°C and crosslinks POE, thus affecting RPM and resin pressing. The output rate cannot exceed the threshold, leading to a resin melting temperature well above 110°C. POE with a higher melt index (i.e., POE with lower viscosity) Lower viscosity and reduced shear heating result in improved processability or through-flow in the extruder. It is known that puts may be present. In this case, both the comparative sample and the sample of the present invention are To ensure excellent processability of the compound, it is designed to have a relatively high melt index. I selected it. However, for high-melt index resins, crosslinked films are typical. These have a relatively low degree of curing. As a result, these high-melt-index resins harden Improving the effectiveness will be important.

[0110] For curing comparison between POEs with different unsaturation levels, equivalent melt index Curing of a POE-containing compound having processability, density, MWD, and comonomer distribution. The effects were investigated (see Table 6). Here, Example 1 was compared to Comparative Example 1 (approximately 14 dg / min melt). Compared to POE with an index, Example 2 was compared to Comparative Example 2 (approximately 30 dg / min). This was compared to POE with a melt index of . The composition of the invention provides an improved (larger) MDR torque change (MH-ML), and "4 The increased gel content after vacuum lamination for "+12 minutes" was clearly demonstrated.

[0111] The results in Table 7 show the curing effect of the sealing film formulations formed from the POE described. Compare. The composition of the present invention (in addition to high unsaturation, has a narrow MWD and a narrow comonomer distribution) The POE (Power over Energy) features improved MDR torque variation (MH-ML), as well as a "4+10 minute" cycle. Best hardness with higher gel content after vacuum lamination and after vacuum lamination of "4+16 minutes". Provides chemical properties. (Higher proportion of vinyl groups to total unsaturation, higher vinyl / vinyl The composition of the present invention (containing POE having a lidene ratio and a narrower comonomer distribution) is Gala It is also noteworthy that it has good adhesion to s.

[0112] [Table 8]

[0113] [Table 9]

Claims

1. The following characteristics: a) Total unsaturation of 0.30 or more / 1000C, b) Molecular weight distribution (MWD) of 3.0 or less, c) TGIC spread parameter B of 8.0 or less １／４ , containing ethylene / α-olefin A composition containing an internomer.

2. The ethylene / α-olefin interpolymer has a density of 0.860 g / cc or more. The composition according to claim 1, having the following characteristics.

3. The ethylene / α-olefin interpolymer has a density of 0.900 g / cc or less. A composition according to claim 1 or claim 2, having the following characteristics.

4. The aforementioned interpolymer is [(vinyl / 1000C) ＊ (Mn) is 5 × 10 ３ (g The composition according to any one of claims 1 to 3, further comprising a product that is (1 / mol) or more.

5. The aforementioned interpolymer is [(vinyl / 1000C) / (vinylidene / 1000C) The composition according to any one of claims 1 to 4, further comprising the ratio of 2.0 or more. 。

6. The ethylene / α-olefin interpolymer has a vinyl content of 50% or more. A composition according to any one of claims 1 to 5, further comprising the above.

7. The composition further comprises a peroxide and a silane coupling agent, according to claims 1 to 6. The composition described in any one of the items.

8. The composition according to any one of claims 1 to 7, wherein the composition further comprises a crosslinking agent.

9. at least one component formed from the composition according to any one of claims 1 to 8 Articles containing elements.

10. The article according to claim 9, wherein the article is a film.

11. The article according to claim 9, wherein the article is a solar cell module.

12. In a solution polymerization process for preparing ethylene / α-olefin / interpolymer The process involves, in a single reactor, at a reactor temperature of 150°C or higher, ethylene, Polymerization of a reaction mixture containing an α-olefin, a solvent, and a metal complex selected from a) below. This includes doing a) Biphenylphenol metal complex selected from the following structure 1: 【Chemistry 1】 M is either Zr or Hf, and the metal has a formal oxidation state of +2, +3, or +4. 、 n is 0, 1, or 2. When n is 1, X is a monosect ligand or a bisect ligand. When n is 2, each X is an independently selected monodentate ligand. The aforementioned metal complex is charge-neutral overall. -Z １ - and -Z ２ Each of these is independently -O-, -S-, and -N(R) Ｎ ) -, or -P(R) Ｐ ) - Selected from, R １ and R ８ each independently represents -H, (C １ ~C ４０ )-hydrocarbyl, (C １ ~C ４０ ) Heterohydrocarbyl, -Si(R Ｃ ) ３ ,-Ge(R Ｃ ) ３ , -P(R Ｐ ) ２ , -N(R Ｎ ) ２ 、-OR Ｃ 、-SR Ｃ 、-NO ２ 、-CN、-CF ３ 、R Ｃ S(O)-、 R Ｃ S(O) ２ -、(R Ｃ ) ２ C=N-、R Ｃ C(O)O-、R Ｃ OC(O)-、R Ｃ C (O)N(R)-, (R Ｃ ) ２ NC(O)-, halogen, radical having formula (I), formula Selected from the group consisting of radicals having formula (II) and radicals having formula (III) 、 【Chemistry 2】 In the formula, R ３１～３５ , R ４１～４８ , and R ５１～５９ Each of them is independent of (C １ ~C ４０ ) Hydrocarbyl, (C １ ~C ４０ ) Heterohydrocarbyl, -Si(R Ｃ ) ３ 、-Ge(R Ｃ ) ３ 、-P(R Ｐ ) ２ 、-N(R Ｎ ) ２ 、-N=CHR Ｃ 、-OR Ｃ 、- SR Ｃ 、-NO ２ 、-CN、-CF ３ 、R Ｃ S(O) - R Ｃ S(O) ２ -、(R Ｃ ) ２ C=N-、R Ｃ C(O)O-、R Ｃ OC(O)-、R Ｃ C(O)N(R Ｎ )-、(R Ｃ ) ２ Selected from NC(O)-, halogen, or -H, R ２～７ , R ９～１６ Each of them is independent of (C １ ~C ４０ ) Hydrocarbyl, (C １ ~C ４０ ) Heterohydrocarbyl, -Si(R Ｃ ) ３ ,-Ge(R Ｃ ) ３ , -P(R Ｐ ) ２ 、-N(R Ｎ ) ２ 、-N=CHR Ｃ 、-OR Ｃ 、-SR Ｃ 、-NO ２ 、-CN、-C F ３ 、R Ｃ S(O)-、R Ｃ S(O) ２ -、(R Ｃ ) ２ C=N-、R Ｃ C(O)O-、R Ｃ OC(O)-, R Ｃ C(O)N(R) Ｎ ) -, (R Ｃ ) ２ NC(O)-, halogen, or - Selected from H, L is (C １ ~C ４０ ) hydrocarbylene or (C １ ~C ４０ ) heterohydrocarbyl It is Len, and the above (C １ ~C ４０ ) Hydrocarbylene has two Z groups (L) in structure 1. It contains a linker backbone of 1 to 10 carbon atoms that connects (which are bonded together). Having a portion, or the (C １ ~C ４０ ) Heterohydrocarbylene in structure 1 It has a portion containing a linker main chain of 1 to 10 atoms that connects the two Z groups. , the above (C １ ~C ４０ ) The 1 to 10 atoms of the heterohydrocarbylene phosphorus Each of the 1 to 10 atoms in the Kerr main chain is independently a carbon atom or a heteroatom group. Each heteroatom group is independently O, S, S(O), S(O) ２ , Si(R Ｃ ) ２ , Ge (R Ｃ ) ２ , P(R Ｃ ), or N (R Ｃ ) and each R in structure 1 Ｃ , R Ｐ , and R Ｎ (C １ ~C ３０ ) Hydrocarbyl, (C １ ~C ３０ ) Heterohydrocal A solution polymerization process that is either a birch or -H polymerase.

13. The above process is carried out at a reactor temperature of 150°C or higher, yielding 2.5 × 10 ６ The overall catalyst Claim 1, having an efficiency [(grams of interpolymer) per (grams of total catalyst metal)] The process described in section 2.

14. The process involves 0.860 to 0.900 g / cc of ethylene / α-olefin in The terpolymer density is 2.5 × 10 ６ The overall catalytic efficiency [(total catalyst metal grams) per...] The process according to claim 12 or 13, comprising [a (interpolymer gram)].

15. TGIC broadening parameters of a polymer composition containing one or more olefin polymers Ta B １／ｘ The method for making the decision involves the following steps: a) Dissolving the polymer composition in an organic solvent to form a polymer solution, b) At least a portion of the polymer solution is a color containing a support material including graphite. Steps to inject into the mu c) A step of cooling the support material at a rate of 0.1°C / min or more. d) Raise the temperature of the support material to allow the polymer (multiple polymers may be used) of the polymer composition to rise. ) a step of eluting, e) Step of generating a "dwi / dT vs temperature" profile, f) Regarding the maximum height of the profile (dwi / dTi vs temperature), A step of calculating the width of the profile at 1 / x (x > 1), g) A step of determining the temperature (Tp) at the maximum height of the profile, h) From EICOSANE / iPP / HDPE reference, (at an elution temperature of 150.0°C) Calculate the peak width of HDPE at 1 / x of the HDPE peak height (peak width at 1 / x). The step is to analyze the criteria by TGIC according to steps a) to g). The steps to be performed, i) The above B １／ｘ The following formula: [Math 1] A method that includes the step of calculating based on.

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