DoE use in FKM custom compounding.Custom compounding requires the development of materials that must meet the physical property criteria criteria (krītēr´ē  ),n. defined by the customer and their application. Often the physical property criteria are competing with one another and it may be difficult to identify the optimum compound to meet all requirements. In addition, it is often necessary to develop the solution in a very short amount of time. The design of experiments, or experimental design, is one tool available to the compounder to address these requirements. Designed experiments can generate predictive models and greatly increase the compounder' s understanding of how the input variables (e.g., compound ingredients) affect the outputs (e.g., physical properties). Mathematical techniques may be used in conjunction conjunction, in astronomy conjunction, in astronomy, alignment of two celestial bodies as seen from the earth. Conjunction of the moon and the planets is often determined by reference to the sun. with the designed experiment to further enhance our understanding of the observed ob·serve v. ob·served, ob·serv·ing, ob·serves v.tr. 1. To be or become aware of, especially through careful and directed attention; notice. 2. phenomena. Many types of experimental designs have been developed. A thorough review of these designs is beyond the scope of this article, however, it should be noted that these designs each have their unique strengths in their application to experimental challenges. One characteristic that they all share is the need for the experimenter to take the time to design a test plan, execute To run a program, which causes the computer to carry out its instructions. See executable code, instruction and EXE file. execute - execution the test plan and analyze an·a·lyze v. 1. To examine methodically by separating into parts and studying their interrelations. 2. To separate a chemical substance into its constituent elements to determine their nature or proportions. 3. the results. These test plans can be quite involved, requiring dozens of test measurements and man-hours for design, execution and analysis. Furthermore, if a designed experiment is halted prior to completing the design matrix, there is a significant probability probability, in mathematics, assignment of a number as a measure of the "chance" that a given event will occur. There are certain important restrictions on such a probability measure. that the data will not generate a useful model. A compounder can use his or her experience to reduce the scope of the experimental design. For example, when given requirements of maximum compression compression, external stress applied to an object or substance, tending to cause a decrease in volume (see pressure). Gases can be compressed easily, solids and liquids to a very small degree if at all. set and minimum elongation elongation, in astronomy, the angular distance between two points in the sky as measured from a third point. The elongation of a planet is usually measured as the angular distance from the sun to the planet as measured from the earth. , the compounder may use his knowledge of the compound to limit his input variables to those few ingredients known to affect cross-link cross-link (kros´link?) a covalent bond formed between polymer chains, either within or across chains. density to develop an optimized solution. Simplified sim·pli·fy tr.v. sim·pli·fied, sim·pli·fy·ing, sim·pli·fies To make simple or simpler, as: a. To reduce in complexity or extent. b. To reduce to fundamental parts. c. experimental designs can be quickly completed to give compounds that meet multiple physical property requirements in a limited timeframe. An alternate alternate /al·ter·nate/ (awl´ter-nit) 1. following in turns. 2. pertaining to every other one in a series. 3. occurring in place of another; acting as a substitute. to experimental design is to run a series of experiments changing one factor at a time (OFAAT). These are credible alternatives but can lead to misleading results, especially when interactions are present. Nonetheless, they can prove useful to improve understanding and screen ideas. A compounder may also employ a "silver bullet silver bullet - magic bullet " approach, using past knowledge to establish trial recipes Recipes by category Albanian cuisine
http://ecrc.de/facile/facile_home.html. ["Facile: A Symmetric Integration of Concurrent and Functional Programming", A. Giacalone et al, Intl J Parallel Prog 18(2):121-160, Apr 1989]. and quick, this technique will show only whether a particular compound meets the requirements and provides limited direction to the experimenter. Experimental In each example, a simple designed experiment, or series of experiments, was run to determine if an optimum compound could be designed to meet multiple physical property requirements. In most cases, a simple 2 x 2 block design was employed. Test compounds were prepared using commercially available ingredients and mixed on a 6" x 13" laboratory mill. Test samples were cured 10 minutes at 177[degrees]C in a lab press and post cured as noted. Physical testing was performed similar to the following test procedures: * ASTM ASTM abbr. American Society for Testing and Materials D-395-03, rubber property--compression set; * ASTM D-412-98a, vulcanized rubber India rubber, vulcanized. - Knight. See also: Vulcanize and thermoplastic A polymer material that turns to liquid when heated and becomes solid when cooled. There are more than 40 types of thermoplastics, including acrylic, polypropylene, polycarbonate and polyethylene. elastomers--tension; * ASTM D-2084-01, vulcanization vulcanization (vŭl'kənəzā`shən), treatment of rubber to give it certain qualities, e.g., strength, elasticity, and resistance to solvents, and to render it impervious to moderate heat and cold. using oscillating os·cil·late intr.v. os·cil·lat·ed, os·cil·lat·ing, os·cil·lates 1. To swing back and forth with a steady, uninterrupted rhythm. 2. disk cure meter meter, unit of measure meter, abbr. m, fundamental unit of length in the metric system. The meter was originally defined as 1/10,000,000 of the distance between the equator and either pole; however, the original survey was inaccurate and the meter was later ; * ASTM D-624-00, tear strength of conventional vulcanized rubber and thermoplastic elastomers Thermoplastic elastomers (TPE), sometimes referred to as thermoplastic rubbers, are a class of copolymers or a physical mix of polymers (usually a plastic and a rubber) which consist of materials with both thermoplastic and elastomeric properties. ; * ASTM D-2240-05, rubber property--durometer hardness; and * ASTM D-6204-05, measurement of unvulcanized Adj. 1. unvulcanized - (used of rubber) not subjected to the process of vulcanization unvulcanised unprocessed - not altered from an original or natural state; "unprocessed commodities" rheological rhe·ol·o·gy n. The study of the deformation and flow of matter. rhe  o·log properties using rotorless shear shear: see strength of materials. Shear A straining action wherein applied forces produce a sliding or skewing type of deformation. rheometers. In each example, the test program was adjusted to meet each experiment's requirements. In most cases, the individual experiments were completed within one week. Results and discussion Example 1 In this example, the customer requested an 85 durometer Du`rom´e`ter n. 1. An instrument for measuring the degree of hardness; especially, an instrument for testing the relative hardness of steel rails and the like. "GF" compound (ASTM D-2000 classification) with good rubber-to-metal bonding and optimum tear strength. Metal oxide oxide, chemical compound containing oxygen and one other chemical element. Oxides are widely and abundantly distributed in nature. Water is the oxide of hydrogen. Silicon dioxide is the major component of sand and quartz. choice is known to affect rubber-to-metal bonding, and carbon black choice affects tear strength of fluoroelastomer compounds. A 2 x 2 block experiment was designed to demonstrate the effect of the two factors: metal oxide and carbon black. The experimental design, recipes and results are shown in table 1. Compound #3 demonstrated the best tear strength and good overall properties, and was sampled to the customer for evaluation. The customer stated that the compound demonstrated good bonding performance in their process. Example 2 In this example, the customer provided a recipe and a set of physical property targets. The compound did not meet the physical property targets in initial testing. Using their recipe, we conducted a designed experiment to study the effect of post cure time and temperature on physical properties. The design was a 2 x 2 block design with a center point. Times (6 and 24 hours) and temperatures (177 and 232[degrees]C) were chosen to encompass the range of post cure conditions reported for comparable FKM FKM Fluoroelastomer FKM Fogarty Klein Monroe (Houston, Texas) FKM Field Kitchen, Modular compounds. A sixth point (12 hours at 121[degrees]C) was added as indicated by the customer. The principal objective of the study was to increase the 100% modulus See modulo. result, with a secondary objective to meet the physical property targets. The design and results are summarized in table 2. Since the study objective was to maximize In a graphical environment, to enlarge a window to the full size of the screen. See Win Maximize windows. modulus, graphical techniques were used in place of strict mathematical analysis Analysis has its beginnings in the rigorous formulation of calculus. It is the branch of mathematics most explicitly concerned with the notion of a limit, whether the limit of a sequence or the limit of a function. . The following trends were noted: * Temperature had a greater effect than time; * tensile strength tensile strength Ratio of the maximum load a material can support without fracture when being stretched to the original area of a cross section of the material. When stresses less than the tensile strength are removed, a material completely or partially returns to its and elongation exceeded their property objectives at all test conditions; * elongation decreased with increasing post cure temperature; * compression set was above the property target and was surprisingly unaffected by post cure conditions; * none of the modulus results met the property objective for this compound; and * modulus seemed to trend upward with increasing post cure temperature. Post cure conditions were unable to bring the compound into compliance with the customers' property objectives. It is clear that another factor will need to be studied to meet customer property targets. Example 3 In this example, the customer requested a compound with a set of physical property targets which included 100% modulus and elongation at break values that can be high for an FKM compound. In addition, the customer specified spec·i·fy tr.v. spec·i·fied, spec·i·fy·ing, spec·i·fies 1. To state explicitly or in detail: specified the amount needed. 2. To include in a specification. 3. that the compound must be at least 60% polymer polymer (pŏl`əmər), chemical compound with high molecular weight consisting of a number of structural units linked together by covalent bonds (see chemical bond). , limiting the recipe to 166.67 parts per hundred rubber (pphr). Cure conditions were not specified and evaluations were completed after both press cure and post cure conditions in an attempt to satisfy all requirements. A variety of experimental techniques Experimental research designs are used for the controlled testing of causal processes. The general procedure is one or more independent variables are manipulated to determine their effect on a dependent variable. was employed to address this customer's needs. The first designed experiment in this development program was a 2-factor, 2-level factorial factorial For any whole number, the product of all the counting numbers up to and including itself. It is indicated with an exclamation point: 4! (read “four factorial”) is 1 × 2 × 3 × 4 = 24. design where the factors were polymer and cure type. The experimental design, recipes and physical property results are summarized in table 3. Adding terpolymer ter·pol·y·mer n. A polymer that consists of three distinct monomers. [Latin ter, thrice; see trei- in Indo-European roots + polymer.] FKM (Viton B) to the recipe increased durometer and specific gravity specific gravity, ratio of the weight of a given volume of a substance to the weight of an equal volume of some reference substance, or, equivalently, the ratio of the masses of equal volumes of the two substances. and decreased tensile strength. Changing curative curative /cur·a·tive/ (kur´ah-tiv) tending to overcome disease and promote recovery. cu·ra·tive adj. 1. Serving or tending to cure. 2. type had little effect on physical properties. None of the compounds tested met the durometer target, necessitating additional study. The designed experiment showed that little improvement towards the property targets could be made with changes in polymer and cure type, so a "silver bullet" trial was established with the original polymer, cure type and adjusted filler fill·er 1 n. One that fills, as: a. Something added to augment weight or size or fill space. b. A composition, especially a semisolid that hardens on drying, used to fill pores, cracks, or holes in wood, plaster, packages in hopes of quickly obtaining a satisfactory solution. The two compounds in this trial and their properties are included in table 4. While both compounds were closer to the modulus and elongation requirements than the compounds shown in table 3, neither compound satisfied all requirements. Since a satisfactory solution had not been reached, a single factor (mineral filler), screening experiment was run to determine which mineral fillers may offer an improved balance of properties to meet these requirements. Mineral fillers commonly used in FKM compounding were compared at equal loading, and high surface area silicas were included at lower loading. The filler study is summarized in table 5. Some of the fillers interrupted in·ter·rupt v. in·ter·rupt·ed, in·ter·rupt·ing, in·ter·rupts v.tr. 1. To break the continuity or uniformity of: Rain interrupted our baseball game. 2. the crosslinking reaction of this compound and additional curatives were added to yield compounds that would cure in 10 minutes at 177[degrees]C. As expected, none of the compounds met all of the physical property requirements. However, the experiment did show which fillers would give increased modulus and how the other properties would be affected. A 3-factor, 2-level factorial experiment fac·to·ri·al experiment n. An experimental design in which two or more series of treatments are tried in all combinations. factorial experiment see factorial experiment. was then run to more closely examine the filler effects on compound properties. The factors were: silica silica or silicon dioxide, chemical compound, SiO2. It is insoluble in water, slightly soluble in alkalies, and soluble in dilute hydrofluoric acid. Pure silica is colorless to white. surface area, curative amount and the presence of a silane silane or silicon hydride Any of a series of inorganic compounds of silicon and hydrogen with covalent bonds and the general chemical formula SinH(2n + 2). treatment on the primary mineral filler, wollastonite wol·las·ton·ite n. A white to gray mineral, essentially CaSiO3, found in metamorphic rocks and used in ceramics, paints, plastics, and cements. [After William Hyde Wollaston. . The experimental design, compound recipes and physical property results are included in table 6. While none of the compounds met all physical property requirements at a given cure condition, some of the trials were close and the data allows us to quantify Quantify - A performance analysis tool from Pure Software. the impact of each input variable. Compound E7 met the modulus and tensile strength requirements and demonstrated good elongation properties. Compound F2 (table 7) was based on Compound E7, but used an alternate source for the high surface area silica and an adjustment in the wollastonite content to meet the durometer target. This compound met all physical property targets except elongation at break and the customer accepted the compound for molding molding, in architecture, furniture, and decorative objects, a surface or group of surfaces of projecting or receding contours. A molding may serve as a defining element, terminating a unit or an entire composition (e.g. trials and product evaluation. Example 4 Most FKM polymers, when compounded, have durometer values of 50 or greater. Recipes to meet a 45 durometer target will contain very little filler, and most of the filler will be the acid acceptors needed for the curing reaction. The two acid acceptors commonly used in FKM compounding are calcium hydroxide calcium hydroxide, Ca(OH)2, colorless crystal or white powder. It is prepared by reacting calcium oxide (lime) with water, a process called slaking, and is also known as hydrated lime or slaked lime. and high activity magnesium oxide magnesium oxide: see magnesia. . A 2-factor, 3-level experiment was conducted to demonstrate the effects of the two metal oxides on physical properties in a 45-durometer FKM compound. This experiment is summarized in table 8. Compound B did not fully cure after 10 minutes at 177[degrees]C. Higher filler content in compounds D and E raised the compound durometer above the 45-durometer target range (45 [+ or -] 5). Data from the remaining compounds can be employed to address specific requirements for a 45 durometer FKM compound. Example 5 In this example, we received a set of physical property targets for a 70 durometer TFE/P based compound. The first compound samples demonstrated low specific gravity and physical properties outside the target ranges. A 2-factor, 2-level design was employed to determine the effect of polymer viscosity and curative level in recipes with a revised filler content. The design, recipes and results are shown in table 9. The results provided a quantitative quantitative /quan·ti·ta·tive/ (kwahn´ti-ta?tiv) 1. denoting or expressing a quantity. 2. relating to the proportionate quantities or to the amount of the constituents of a compound. model of the effect of each of the input factors. Compound B4 met durometer, specific gravity and tensile strength targets while exceeding the elongation target range and being slightly below the targets for modulus. This compound will be the starting point Noun 1. starting point - earliest limiting point terminus a quo commencement, get-go, offset, outset, showtime, starting time, beginning, start, kickoff, first - the time at which something is supposed to begin; "they got an early start"; "she knew from the for further samples and study. Summary A variety of experimental tools is available to the compounder to optimize optimize - optimisation recipes to meet customer needs. Simple designed experiments can be used to identify compound recipes that meet multiple, often competing, requirements. Five examples were shown where designed experiments assisted compound development. Gary Gary, city (1990 pop. 116,646), Lake co., NW Ind., a port of entry on Lake Michigan; inc. 1909. Gary was founded by the U.S. Steel Corporation, which purchased the land in 1905 and landscaped it for a city. D. D'Abate (gdabate@rex-hide.com) Pinnacle pinnacle (pĭn`ĭkəl), minor architectural motif of vertical tapering shape, usually crowning a pier, buttress, or gable. Although sometimes it appears in Renaissance design, as in the Certosa di Pavia, it is almost exclusively a medieval Elastomeric Technology
Table 1--experimental design and results from example 1
Compound 1 2 3 4
Experimental design
factors/levels
Metal oxide -1 -1 1 1
Carbon black -1 1 -1 1
Ingredient
Viton GF600-S 90 90 90 90
Viton GF 10 10 10 10
Carbon black--N990 75 35 75 35
Carbon black--N550 20 20
Zinc oxide 911-c 3 3
Elastomag 170 3 3
TAIC-DLC, 72% active 1.5 1.5 1.5 1.5
Varox DBPH-50 1.5 1.5 1.5 1.5
Total pphr 181 161 181 161
Press cure 90' @
154[degrees]C
Durometer A hardness 85 84 86 85
Specific gravity 1.89 1.891 1.881 1.882
Tensile strength, MPa 13.1 17.5 15.3 21.0
Elongation, % 178 176 183 177
100% modulus, MPa 8.6 9.2 10.6 11.9
Tear Die C, N/m 27.3 26.8 28.0 23.5
ODR @ 177[degrees]C
ML, dN-m 22.58 23.76 27.09 26.13
MH, dN-m 141.6 134.7 150.0 147.9
Ts2, min. 0.65 0.85 0.71 0.85
Tc90, min. 2.82 3.99 3.03 4.25
Effect calculations
Metal Cblk
oxide
+1 -1
-0.009 +0.001
+2.8 +5.1
+3 -4
+2.3 +0.9
-1.3 -2.5
+3.44 +0.11
+10.80 -4.48
+0.03 +0.17
+0.23 +1.19
Table 2--post cure study
Post cure hours 12 6 24 12 6
Post cure temp., [degrees]C 121 177 177 204 232
Durometer A hardness 68 68 68 69 68
Specific gravity 1.847 1.848 1.852 1.854 1.857
Tensile strength, MPa 15.5 13.4 14.4 14.5 13.9
Elongation at break, % 608 531 560 498 492
100% modulus, MPa 2.15 1.90 1.84 2.29 1.85
* Compression set, % 25.3 25.9 26.0 26.9 25.0
Post cure hours 24 Objec-
Post cure temp., [degrees]C 232 tives
Durometer A hardness 69 65~75
Specific gravity 1.866 1.85
Tensile strength, MPa 15.5 12.4-15.2
Elongation at break, % 465 [greater than or
equal to] 300
100% modulus, MPa 2.15 [greater than or
equal to] 2.41
* Compression set, % 23.9 [less than or
equal to] 15
* Compression set measured after 22 hrs. at 70[degrees]C
Table 3--two-factor, two-level factorial design in green FKM compound
Experimental design: Factors
Lo (-) Hi (+)
Polymer A A A/B
Cure type VC50 VC30/20
Experimental design:
Coded trials
Polymer -1 1 -1 1
Cure type -1 -1 1 1
Recipes, pphr Recipes, pphr
Description X 1602B1 X 1602B2 X 1602B3 X 1602B4
Viton AHV 40 40 40
Viton B600 40 40
Viton A601c 60 60
Viton A500 56.5 16.5
Viton VC-30 2.3 2.3
Viton VC-20 1.2 1.2
NYAD 400 50 50 50 50
(wollastonite)
Akrochem E2616 5 5 5 5
green powder
Carbon black--N550 1 1 1 1
Calcium hydroxide 3 3 3 3
Elastomag 170 6 6 6 6
Struktol WS280 powder 1 1 1 1
Total pphr 166 166 166 166
Press cure 10' @
177[degrees]C
Durometer A hardness 73 73 73 73
Specific gravity 2.113 2.133 2.121 2.138
Tensile strength, MPa 8.85 7.99 8.74 7.76
Elongation at break, % 390 432 447 556
100% modulus, MPa 3.27 2.83 2.99 2.98
Post cured 4 hrs. @
204[degrees]C
Durometer A hardness 74 73 74 75
Specific gravity 2.125 2.137 2.123 2.141
Tensile strength, MPa 12.22 8.08 11.46 9.36
Elongation at break, % 331 285 321 334
100% modulus, MPa 5.70 4.64 5.65 5.70
Post cured 16 hrs. @
232[degrees]C
Durometer A hardness 73 74 73 75
Specific gravity 2.131 2.147 2.13 2.145
Tensile strength, MPa 10.36 9.10 10.71 8.76
Elongation at break, % 219 210 245 272
100% modulus, MPa 6.10 5.65 5.69 5.38
Targets
Durometer A hardness 80 [+ or -] 3
Specific gravity
Tensile strength, MPa [greater than or
equal to] 11.0
Elongation at break, % [greater than or
equal to] 350
100% modulus, MPa [greater than or
Post cured 4 hrs. @ equal to] 6.89
204[degrees]C
Durometer A hardness 80 [+ or -] 3
Specific gravity
Tensile strength, MPa [greater than or
equal to] 11.0
Elongation at break, % [greater than or
equal to] 350
100% modulus, MPa [greater than or
Post cured 16 hrs. @ equal to] 6.89
232[degrees]C
Durometer A hardness 80 [+ or -] 3
Specific gravity
Tensile strength, MPa [greater than or
equal to] 11.0
Elongation at break, % [greater than or
equal to] 350
100% modulus, MPa [greater than or
equal to] 6.89
DOE effect calculations
Polymer Cure type
0 0
0.0185 0.0065
-0.9136 -0.1689
75.5 90.5
-0.2206 -0.0689
0 1
0.015 0.001
-3.1233 0.2551
-16.5 19.5
-0.5033 0.5033
1.5 0.5
0.0155 -0.0015
-1.603 0.0034
9 44
--0.3758 --0.3413
Table 4--silver bullet trial--green FKM, compound
Description X1602C1 X1602C2
Viton AHV 40 40
Viton A601c 60 60
Ultrasil 880 20 10
NYAD 400 20 20
Wollastocoat 10012 10 20
Akrochem E2616 5
green powder 5
Carbon black--N550 1 1
Calcium hydroxide 3 3
Elastomag 170 6 6
Struktol WS280 Powder 1 1
Total pphr 166 166
Press cure 10' @ Targets
177[degrees]C
Durometer A hardness 74 71 80 [+ or -] 3
Specific gravity 2.032 2.078
Tensile strength, MPa 9.24 10.38 [greater than or
equal to] 11.0
Elongation at break, % 452 331 [greater than or
equal to] 350
100% modulus, MPa 3.56 3.70 [greater than or
Post cured 4 hrs. equal to] 6.89
@ 204[degrees]C
Durometer A hardness 78 75 80 [+ or -] 3
Specific gravity 2.029 2.076
Tensile strength, MPa 13.98 14.55 [greater than or
equal to] 11.0
Elongation at break, % 244 211 [greater than or
equal to] 350
100% modulus, MPa 5.68 5.81 [greater than or
Post cured 16 hrs. @ equal to] 6.89
232[degrees]C
Durometer A hardness 79 76 80 [+ or -] 3
Specific gravity 2.034 2.083
Tensile strength, MPa 13.64 13.97 [greater than or
equal to] 11.0
Elongation at break, % 217 192 [greater than or
equal to] 350
100% modulus, MPa 5.94 6.19 [greater than or
equal to] 6.89
Table 5--screening fillers in green FKM compound
Description X1602- D1 D2 D3 D4
Viton AHV 40 40 40 40
Viton A601c 60 60 60 60
NYAD 400 50
Atomite whiting 50
Mistron vapor 50
HiSil 532 50
Cab-O-Sil M7D
Degussa FK 160
Akrochem E2616 Green Powder 5 5 5 5
Carbon black--N550 1 1 1 1
Calcium hydroxide 3 3 3 3
Elastomag 170 6 6 6 6
Struktol WS280 Powder 1 1 1 1
Total pphr 166 166 166 166
Repair by adding curative so that sample would cure
Viton VC30 4.0 3.5
Viton VC20 2.0 1.75
Viton RCR-7014 0.2 0.175
ODR @ 177[degrees]C
MH-ML, dN-m 68.5 70.4 124.6 115.0
ML (first pass), dN-m 23.2 25.8 14.2 47.6
Press cure 10' @
177[degrees]C
Durometer A hardness 73 73 90 92
Specific gravity 2.123 2.09 2.068 1.915
Tensile strength, MPa 8.0 10.1 17.6 13.3
Elongation at break, % 432 497 143 162
100% modulus, MPa 2.72 2.74 16.11 11.36
Post cured 4 hr. @
204[degrees]C
Durometer A Hardness 71 72 90 94
Specific gravity 2.127 2.09 2.074 2.074
Tensile strength, MPa 9.0 12.8 22.6 17.4
Elongation at break, % 262 206 91 79
100% modulus, MPa 4.71 5.74 -- --
Description D5 D6
Viton AHV 40 40
Viton A601c 60 60
NYAD 400
Atomite whiting
Mistron vapor
HiSil 532
Cab-O-Sil M7D 30
Degussa FK 160 30
Akrochem E2616 Green Powder 5 5
Carbon black--N550 1 1
Calcium hydroxide 3 3
Elastomag 170 6 6
Struktol WS280 Powder 1 1
Total pphr 146 146
Repair by adding curative so that sample would cure
Viton VC30 8.0
Viton VC20 4.35
Viton RCR-7014 0.7
ODR @ 177[degrees]C
MH-ML, dN-m 173.4 --
ML (first pass), dN-m 68.4 58.7
Press cure 10' @ Targets
177[degrees]C
Durometer A hardness 94 Did 80 [+ or -] 3
Specific gravity 1.915 not
Tensile strength, MPa 16.7 cure [greater than or
equal to] 11.0
Elongation at break, % 74 [greater than or
equal to] 350
100% modulus, MPa -- [greater than or
Post cured 4 hr. @ equal to] 6.89
204[degrees]C
Durometer A Hardness 94 80 [+ or -] 3
Specific gravity 1.915
Tensile strength, MPa 18.7 [greater than or
equal to] 11.0
Elongation at break, % 27 [greater than or
equal to] 350
100% modulus, MPa -- [greater than or
equal to] 6.89
Table 6--3 factor, 2 level factorial design in green FKM
Experimental design Level
Variable - +
Silica surface area HiSil 532 CabOSil
BPAF amount +0 +2
Silane NYAD Coated
Experimental design--
Coded trials
Factor: Silica -1 -1 1 1 -1 -1
Factor: BPAF cure -1 1 -1 1 -1 1
Factor: Aminosilane -1 -1 -1 -1 1 1
Recipes, pphr
Description x1602 E1 E2 E3 E4 E5 E6
Viton AHV 39 39 39 39 39 39
Viton A601c 60 60 60 60 60 60
VC 20 1 1 1 1 1 1
VC30 2 2 2
NYAD 400 30 30 30 30
Wollastocoat 10012 30 30
HiSil 532 10 10 10 10
Cab-O-Sil M7D 10 10
Akrochem E2616 5 5 5 5 5 5
green powder
Carbon black--N550 1 1 1 1 1 1
Calcium hydroxide HP 3 3 3 3 3 3
Elastomag 170 6 6 6 6 6 6
Struktol WS280 powder 1 1 1 1 1 1
Total pphr 156 158 156 158 156 158
ODR @ 177[degrees]C
ML, dN-m 30.2 21.1 26.9 22.1 28.1 23.6
MH, dN-m 84.7 145.7 43.3 90.7 96.8 155.6
Ts2, min. 0.81 1.77 2.39 3.27 1.06 2.51
Tc90, min. 3.51 3.33 6.06 8.35 3.97 5.09
CRI (90/2) 37.0 64.1 27.2 19.7 34.4 38.8
Press cure 10'@
177[degrees]C
Durometer A 64 77 77 80 75 78
Specific gravity 2.037 2.033 2.042 2.046 2.041 2.034
Tensile strength, MPa 10.1 10.3 6.6 11.5 13.1 16.6
Elongation at break, % 425 257 635 353 218 168
100% modulus, MPa 3.54 5.11 3.68 5.06 5.76 10.45
Post cured 4 his. @
204[degrees]C
Durometer A 76 78
Specific gravity 2.037 2.032
Tensile strength, MPa 14.7 19.8
Elongation at break, % 161 127
100% Modulus, MPa 8.00 14.87
Post cured 16 his. @
232[degrees]C
Durometer A 76 80 81 84 77 78
Specific gravity 2.046 2.039 2.036 2.06 2.042 2.036
Tensile strength, MPa 13.5 17.3 10.5 18.3 14.9 21.2
Elongation at break, % 197 132 236 168 156 116
100% modulus, MPa 7.07 12.89 7.06 11.74 8.20 17.56
Experimental design--
Coded trials
Factor: Silica 1 1
Factor: BPAF cure -1 1
Factor: Aminosilane 1 1
Recipes, pphr
Description x1602 E7 E8
Viton AHV 39 39
Viton A601c 60 60
VC 20 1 1
VC30 2
NYAD 400
Wollastocoat 10012 30 30
HiSil 532
Cab-O-Sil M7D 10 10
Akrochem E2616 5 5
green powder
Carbon black--N550 1 1
Calcium hydroxide HP 3 3
Elastomag 170 6 6
Struktol WS280 powder 1 1
Total pphr 156 158
ODR @ 177[degrees]C
ML, dN-m 26.4 23.9
MH, dN-m 44.4 92.4
Ts2, min. 2.45 3.58
Tc90, min. 6.76 9.01
CRI (90/2) 23.2 18.4
Press cure 10'@ Targets
177[degrees]C
Durometer A 79 82 80 [+ or -] 3
Specific gravity 2.05 2.046
Tensile strength, MPa 9.3 16.3 11.0 min.
Elongation at break, % 540 233 350 min.
100% modulus, MPa 4.72 8.39 6.89 min.
Post cured 4 his. @
204[degrees]C
Durometer A 80 84 80 [+ or -] 3
Specific gravity 2.05 2.045
Tensile strength, MPa 13.1 21.2 11.0 min.
Elongation at break, % 311 160 350 min.
100% Modulus, MPa 6.61 13.20 6.89 min.
Post cured 16 his. @
232[degrees]C
Durometer A 81 84 80 [+ or -] 3
Specific gravity 2.05 2.052
Tensile strength, MPa 13.7 20.6 11.0 min.
Elongation at break, % 252 152 3,50 min.
100% modulus, MPa 7.18 13.24 6.89 min.
DoE effect calculus
Silica BPAF Silane
-1.85 -10.48 0.81
-106.0 107.7 12.4
2.77 2.21 0.68
7.14 2.74 1.79
-42.9 9.60 -16.63
12 11 8
0.019 -0.006 0.007
-3 8 8
347 -404 -256
-1 6 6
5 3
0.013 -0.005
0 7
92 -93
-2 7
9.5 5.5 -0.5
0.017 0.007 -0.001
-2 12 5
104 -137 -29
-3 13 4
Table 7--second silver bullet trial in green FKM compound
Recipe, pphr
Ingredient X1602--F2
Viton AHV 39
Viton A601c 60
Viton VC 20 1
Wollastocoat 10012 36
Aerosil R972V 10
Akrochem E2616 green powder
Carbon black--N550 1
Calcium hydroxide 3
Elastomag 170 6
Struktol WS280 powder 1
Total pphr 162
Press cure 10' @ Targets
177[degrees]C
Durometer A hardness 75 80 [+ or -] 3
Specific gravity 2.062
Tensile strength, MPa 14.0 [greater than or
equal to] 11.0
Elongation at break, % 247 [greater than or
equal to] 350
100% modulus, MPa 6.24 [greater than or
Post cured 16 hrs. @ equal to] 6.89
232[degrees]C
Durometer A hardness 78 80 [+ or -] 3
Specific gravity 2.088
Tensile strength, MPa 16.4 [greater than or
equal to] 11.0
Elongation at break, % 182 [greater than or
equal to] 350
100% modulus, MPa 8.02 [greater than or
equal to] 6.89
Table 8--metal oxide level effects in low durometer FKM compouds
Experimental design levels
Calcium hydroxide 0 -1 0 1 0
Elastomag 170 -1 0 0 0 1
Recipes, pphr
Compound A B C D E
Viton A601 c 100 100 100 100 100
Carbon black N550 2 2 2 2 2
Calcium hydroxide 3 0 3 6 3
Elastomag 170 0 3 3 3 6
Total pphr 105 105 108 111 111
ODR @ 177[degrees]C
ML, dN-m 9.7 9.3 9.5 9.0 8.9
MH, dN-m 40.4 16.6 31.2 84.1 86.6
Ts2, min. 5.89 10.51 7.32 3.84 4.52
MDR @ 204[degrees]C
ML, dN-m 1.6 1.4 1.5 1.6 2.3
MH, dN-m 5.6 2.4 4.1 13.6 12.7
Ts2, min. 2.01 >8 2.64 1.04 1.38
Press Cure 10' @ 177[degrees]C
Durometer A hardness 47 45 48 51 52
Specific gravity 1.806 1.648 1.806 1.812 1.823
Tensile strength, MPa 4.42 0.83 5.87 5.02 6.05
Elongation at break, % 570 1,625 831 241 257
100% modulus, MPa 0.93 0.81 0.91 1.39 1.37
Table 9--polymer curative amount effects in TFE/P compound 2 factor,
2 level factorial design
Experimental design
Factor: Polymer: Level -1: Aflas 100 S
Level +1: Aflas 100 S/Aflas 150 P blend
Cure: Level -1: TAIC-DLC 5.5, Vulcup 40 KE 4.0
Level +1: TAIC-DLC 8.33, Vulcup 40 KE 6.0
Material B1 B2 83
Aflas 100-S 100 70 100 70
Aflas 150-P 30 30
Austin Black 15 15 15 15
ExBar W2 10 10 10 10
Trilene 77 2 2 2 2
Akrowax PE-LM 1 1 1 1
Sodium stearate 1 1 1 1
TAIC-DLC, 72% active 5.5 5.5 8.33 8.33
Vulcup 40 KE 4 4 6 6
Total pphr 138.5 138.5 143.3 143.3 Targets
Physical properties
Durometer A hardness 69 69 71 73 65~75
Specific gravity 1.580 1.577 1.574 1.578 1.52~1.62
Tensile strength, MPa 14.5 13.6 13.7 15.2 12.1~16.5
Elongation at break, % 308 333 270 257 175~240
100% modulus, MPa 4.43 3.83 4.94 6.22 6.2
200% modulus, MPa 10.7 9.3 11.1 12.7 13.8
DoE Effects
Polymer Cure
1 3
0.0005 -0.0025
0.286 0.452
6 -57
0.338 1.448
0.114 1.913
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