PE Design 10 Crack
- lucilla-thurgood26
- Aug 13, 2023
- 7 min read
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PE Design 10 Crack
Abstract: A test campaign has been performed to investigate the design of fuselage stiffened panels with different metallic skin concepts (monolithic vs. Metal Laminates), stringer materials and local reinforcements from aluminum, titanium and glass-fiber. Observations were made on the crack growth retardation mechanisms. Bonded doublers and selective reinforcements confirmed to be outstanding tools to improve the damage tolerance properties of structural elements with a minor weight increase.
Typical SEM micrographs to demonstrate the interactions between crack and platelet are shown in Figure 3. Two Vickers indentations are introduced near the platelet, Figure 3(a). The indentation at the left-hand side of the platelet induces four cracks at each indent corner. One crack propagates straight into the platelet then disappears within the platelet. The indentation at the right-hand side of the platelet is much closer to the platelet. This indentation also produces four major cracks in the matrix. One major crack penetrates into the interfacial reaction layer, then forms many small crack branches within the platelet, Figure 3(b).
Table 1 shows the characteristics of each phase within the composites. These values are determined by using the nano-indentation technique at a very small load of 50 mN. No crack was observed at the indent with the optical microscope after the nano-indentation, though micro-cracks may still be formed under the surface [7]. This technique allows us to determine the in situ physical characteristics of each phase in the composite. The measured elastic modulus of Al2O3 and BaTiO3 is 411 GPa and 180 GPa, respectively. The measured value for Al2O3 is close to the values reported previously [8]. The measured elastic modulus of BaTiO3 is 180 GPa, which is higher than the reported values for barium titanate (107120 GPa) [9]. It may be partly due to that the BaTiO3 phase is surrounded by the rigid Al2O3 matrix. It may also be related to the solution of some Al ions into BaTiO3 grain.
The values in Table 1 demonstrate that the hardness of each phase follows the order as Al2O3 > BaAl13.2O20.8 > Ba4(Ti0.833Al0.167)12O27 > BaTiO3. A previous study also indicated that the strength of BaTiO3 is lower than that of Al2O3 [10]. Different from the previous studies on SiC-platelet toughened Al2O3 [2,3,4], the platelets used in the present study are much weaker than the matrix. Furthermore, a dense reaction phase is formed at the interface. However, the work of fracture (Wtotal) as calculated from the area under the stress-strain curve during nano-indentation shows a different trend with that of hardness. From the Table, it suggests that more energy is consumed during the fracturing of the Ba-containing phases. The high fracture energy results from the possible formation of many microcracks.
Table 2 shows the residual stress in the alumina phase of composites. A very small residual stress is present in the monolithic alumina specimen. Such residual stress may be induced by the surface grinding process. As the platelets were added to form the Ba-containing phases, tensile residual stresses were found in the alumina matrix. It is due to that the thermal expansion coefficient of the Ba-containing phases (11 ppm/K for BaTiO3) [11] is higher than that of alumina (8 ppm/K). Compressive hoop stresses and tensile radial stresses are expected to form at the interface. The crack could deflect around the interface. The nano-indentation analysis demonstrates that the toughening agent used in the present study is softer than that of the matrix. The crack is thus attracted to the platelets because they are elastically softer than the alumina matrix.
The interactions between crack and platelet are demonstrated in Figure 4. As a major crack penetrates into the dense BaAl13.2O20.8 interphase, many crack branches are formed to consume the fracture energy. The crack resistance of the composite is expected to be high. A schematic to demonstrate the toughening behavior is shown in Figure 4.
The composite phase was characterized with a synchrotron X-ray source (Beam-line BL-17B1, National Synchrotron Radiation Research Center, Hsinchu, Taiwan). The diffraction angle (2θ) varied from 20 to 50. The microstructure was observed with SEM (Philips XL-30, Netherlands). Artificial cracks were generated by Vickers hardness tester (AKASHI AVK-A, Japan) under a load of 98N. A nano-indenter (UNAT, ASMEC, Germany) was also used in the present study to determine the elastic modulus, hardness and work-of-fracture of each phase in the composite. The tip was a Berkovich type nano-indenter. The load applied was 50 mN.
"1. A polymer composition for the manufacture of pipes having a design stress of at least 9.0 MPa (PE112) and a slow crack propagation resistance of at least 1000 hours at 4.9 MPa loop [sic] stress at 80ºC temperature, measured according to ISO 13479:1997, comprising 92-99%wt of a bimodal ethylene polymer and 1-8%wt of carbon black, said composition being characterised by having MFR5 measured according to ISO 1133 in the range 0.15 to 0.30 g/10 min and a density in the range 955 to 965 kg/m**(3), said polymer being composed of 42-55%wt of a low molecular weight ethylene homopolymer having MFR2 measured according to ISO 1133 in the range 350 to 1500 g/10 min and 58-45%wt of a high molecular weight copolymer of ethylene with 1-hexene, 4-methyl-1-pentene, 1-octene and/or 1-decene.
- Standard ISO 13479:1997 (D11) which according to claim 1 was used to measure the slow crack resistance at 4.9 MPa only referred to PE 80 and PE 100 resins whereas the patent related to PE112 grade resins. Since D11 stated in Annex A that the test was applicable to other polymer materials, the argument of the patent proprietor that the skilled person would know how to develop test parameters and specifications for PE112 resins was accepted.
- The objection of the opponent that the patent contained no evidence that the pipes prepared exhibited the design stress specified in the claims was itself not supported by any evidence or arguments.
- Although only a single example (example 4) met the product requirements of claim 1 and showed a slow crack propagation resistance of at least 1000 hours, the evidence of the patent as well as the explanation in D16 strongly suggested that the amount of comonomer together with other properties such as MFR5 and density were essential in order to obtain the required combination of design stress and slow crack propagation resistance. The application as filed together with general knowledge of the field put the skilled person into a position to understand these aspects.
"A pipe having a design stress of at least 9.0 MPa (PE112) and a slow crack propagation resistance of at least 1000 hours at 4.9 MPa hoop stress at 80ºC temperature measured according to ISO 13479:1997, formed of a polymer composition comprising 92 to 99 wt.-% of a bimodal ethylene polymer and 1 to 8 wt.-% of carbon black, wherein said polymer composition being characterized by having MFR5 measured according to ISO 1133 in the range of 0.15 to 0.30 g/10min, an FRR21/5 of at least 38, and a density in the range 955 to 965 kg/m**(3), and wherein said bimodal ethylene polymer which has a density of at least 953 kg/m**(3) is composed of 42-55 wt.-% of a low molecular weight ethylene homopolymer having MFR2 measured according to ISO 1133 in the range of 350 to 1500 g/10min and 58-45 wt.-% of a high molecular weight copolymer of ethylene with 1-hexene, 4-methyl-1-pentene, 1-octene and/or 1-decene."
In a communication dated 22 October 2012 the Board set out its preliminary assessment of the case. In particular the Board raised matters relating to Art. 83 EPC querying the nature of the restriction imposed on the claim by the wording "for the manufacture of pipes" having specified properties. The meaning of "design stress" was also referred to, it being noted that the examples did not report this property, nor was there any discussion in the patent of which properties of the composition, or which aspects of the processing affected the "design stress".
(b) Examples 3 and 4 failed to disclose how the polymers had been prepared beyond a teaching that these polymers had been prepared under "slightly different" conditions to those of "Example 1" (by which it was assumed that "Example 2" was meant since Example 1 related to preparation of the catalyst, not to a polymer). The polymer composition of Example 2 had an MFR5 falling outside the scope of the claim but nevertheless resulted in a pipe with the required slow crack propagation resistance at 4.9 MPa hoop stress. In contrast example 3 having a MFR5 value within the scope of the claim resulted in a pipe with slow crack propagation resistance at 4.9 MPa of 965 hours, i.e. below the limit of 1000 hours given in the claim. Arguments of the respondent that 965 hours would be considered as equivalent to 1000 hours by rounding were not consistent with the fact that in the patent the slow crack propagation resistance data was reported to a precision of four significant figures.
(c) Also, the patent in suit provided no guidance how to prepare a polymer resulting in the specified pipe design stress. No example reported the design stress, hence there was no evidence that this requirement of the claims was even met.
The submission of the respondent that the compositions of the examples would inherently result in the required design stress was not credible. In making this argument the respondent had relied on the values of slow crack propagation resistance at 4.9 MPa. However the claim required that the composition resulted in pipes which exhibited both the specified slow crack resistance and the specified design stress, indicating that each of these properties related to different aspects of the composition's characteristics. 2ff7e9595c
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