The term "transparent" and its contrary "opaque" used in said correspondence are unambiguous as Mr Anthony and Mr Koidl, both being experts, made a distinction without any difficulty between a "transparent film" and "semi-transparent" or even "opaque" films. This is also confirmed by the meaning of "transparent" that is found in conventional dictionaries of the English language and the explanations given in document D2, right hand column second paragraph, lines 6 to 8, according to which transparent films let the light through from the infrared to the visible region.
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Document D1a was published on 29 September 1989 (see D30), i.e. after the priority date of the patent in suit, and no indication whatsoever is found anywhere in this document that the samples were transparent in the visible range as are the diamond films claimed in the patent. On the contrary, the microwave assisted CVD technique disclosed in document D1a merely results in an "opaque" or at most in a "semi-transparent" film, rather than in a diamond film exhibiting transparency as claimed. With respect to the process parameters, document D1a is silent about the distance between the heated filament and the substrate. It was, however, found out by the patent proprietor that a strong interdependency exists between the various process parameters i.e. the selected pressure and concentration of methane in the gas mixture, the temperature of the substrate and the filament and the distance between the substrate and the filament. These parameters may be varied only within narrow limits. The properties of the final diamond film are further influenced by the deposition rate and also depend on whether the substrate is arranged vertically or horizontally in the apparatus. Finally, an appropriate substrate material must be selected in order to provide non-adherence of the film to the substrate, i.e. to get a "non-adherent" free-standing diamond film. To this end, molybdenum was found to be a suitable substrate material from which the diamond film separated during the cooling period, whereas silicon was unsuitable since the coefficient of thermal expansion of silicon is close to that of diamond. Thus, a free-standing non-adhering diamond film exhibiting all the properties claimed in the patent is not obtained by the method disclosed in document D1a.
2.4. It is evident from the correspondence and not in dispute between the parties that before the priority date of the patent in suit Mr Anthony of GE sent several samples of free-standing diamond films to Prof. Koidl of Fraunhofer for scientific analysis. A first sample was received by Prof. Koidl in 1988 (see D14a, first page, last paragraph; letter of Mr Anthony to Prof. Koidl, dated December 16, 1988 = enclosure 2 to D14a, second paragraph, last line); from its examination at Fraunhofer the basic physical data were obtained that then were disclosed orally in April 1989 in a lecture at a public conference (see D14, D14a). This first sample was characterized in Mr Anthony's aforementioned letter of 16 December 1988 as being an "unpolished opaque piece" (see D14a enclosure 2; D31c). Enclosed with this letter, Mr Antony forwarded several slices of a second "unpolished semi-transparent" sample to Fraunhofer for investigation and asked to compare these data with those obtained from the previously sent "opaque film". A further diamond strip which, when holding it against the light, exhibited a semi-transparent center between opaque opposing ends was sent to Fraunhofer enclosed with Mr Anthony's letter dated 1 March 1989 (D31d). In response to this letter, Prof. Koidl - after Raman spectroscopy, X-ray diffraction and grain size measurements - held that "transparency (of that last sample) was enhanced by the waveguide-effect of the 110-fibres" (D26 = letter dated 2. April 1989, last two paragraphs).
3.2. Such everyday definitions of transparency are, however, not appropriate to enable in patent claims a clear and unambiguous distinction between the claimed diamond films and those of the prior art. This is even more valid in the present case, since the term "transparency" turns out to be the fundamental key feature. According to the prior art, free-standing diamond films are described as being opaque, brown, greyish, translucent, semi-transparent, or like frosted glass which changes after polishing into "clear". Diamond films can also be in part transparent, namely in the center, whereas the outer ends are opaque. Thus, all grades of transition between the extremes "opaque" on the one hand and "glass-clear" on the other hand do exist. Moreover in its technical definition, the term "transparency" is not confined to the visible part of the electromagnetic wave spectrum, as alleged by the patentee, but also encompasses at least its infrared and ultaviolet regions.
4.3. As to the second question, namely of whether the claimed diamond film was reproducible before the priority date of the patent, the patentee contended for the first time at the oral proceedings before the Opposition Division that the microwave plasma assisted CVD method set out on page 284 of document D1a was not the same as the one applied in the patent in suit and did not lead to transparent diamond films as claimed (see minutes of the oral proceedings before the Opposition Division on 11 May 1998, page 7) 5th full paragraph). In order to disprove this allegation, the opponents OI and OIII submitted comparative tests (documents D15 and D20) in the appeal proceedings. In particular the process parameters selected for performing the experiments HF-MW-1 and 2 described on page 2 of document D15 strictly adhere to those disclosed in document D1a: 1.5 vol% CH4 in H2, 13 mbar = 9.75. torr; tungsten filament temperature 1950 50 C; temperature of the substrate 890 100 C; microwave power 780/750 W, 2.45 GHz; distance between substrate and filament 3 to 8 mm. After removal of the Si-substrate by etching, a 55 µm or 150 µm thick free-standing diamond film was obtained. Due to the polycrystalline structure the diamond films exhibited a rough surface structure but were "transparent to visible light" since a written text could be read through the films (see D15, page 3, paragraph 5.1, Figure 3). The physical parameters obtained from these films comply with those set out in claim 1 of the patent. Based on this evidence it has to be concluded that free-standing polycrystalline diamond films showing a thickness of at least 50 µm and a "transparency" within the meaning encircled in point 3 above could be produced by an expert in the field of CVD.
The question of reproducibility of the claimed diamond films with the method disclosed in D1a and D1b arose for the first time during the oral proceedings before the opposition division, when Mr Anthony, co-author of D1a and D1b, stated that D1b gives an incorrect method (paragraph bridging page 4 and 5 of the minutes) and the method presented in D1b a and D1b is not the GE method (page 7, on top, of the minutes); however, he refused, as he had been instructed by the proprietor, to divulge the method by which the samples forwarded to Prof. Koidl were made, or to say anything about the alleged incorrectness in D1b (top of page 5, bottom of page 6 and fifth full paragraph on page 7 of the minutes). Opponent III reacted to these submissions by referring to Article 113 EPC and asking for an adjournment so that further tests could be made, because he understood that the proprietor's argument which was being heard for the first time is, that the CVD method (presented in D1a and D1b) does not work, in particular leads to non-transparency (page 6, fourth paragraph of the minutes). The proprietor then explicitly contested that there was an enabling prior art disclosure with a hot filament CVD method (page 7, second full paragraph, of the minutes).
To illustrate the usefulness of the current analysis and proposed model for estimating the growth rate of the silver film fabricated by LDSP, simulations for a laser scanning speed of 30 mm/s were made to determine the film thickness after each scan. The computed processing temperature, silver film growth rate, film reflectivity and the accumulated silver film thickness are listed in Table 1. The computed silver line thickness for five, seven and 10 laser scans were compared with experimental results. It can be seen that the computed silver film thickness in each case is close to the measured results. However, it should be noted that the current analysis is valid for an LDSP process carried out within the temperature range investigated, i.e., between 350 and 380 K. Working outside this range might result in the temperature being too low for the formation of a silver film or so high that the substrate would suffer thermal damage. It should also be emphasized that these results and the methodology presented here comes from the first investigation of transport characteristics of a LDSP process. The growth rate of the silver film indeed depends upon coupled thermo-fluidic transport with a chemical reaction, and can be regulated by adjustment of these parameters. It is shown that the proposed semi-empirical model can predict the silver film growth rate in an LDSP process using the parameters of laser power, scanning speed and number of scans. Furthermore, owing to the increased reflectivity of the silver film as its thickness increases, the growth rate decreases gradually to about 10 nm per laser scan after ten scans. It should be noted that this self-controlling effect corresponding to the coupled optical properties and reaction rate of LDSP process can be utilized to control the thickness and uniformity of the metal film. 2ff7e9595c
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