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The apparent strain stability and repeatability of a BCL3 resistance strain gage

Experiments were conducted at NASA-Lewis to study the effect of microstructural instability on the apparent strain stability and reproducibility of a BCL3 resistance strain gage. The resistance drift of the gage at various temperatures in the phase transition temperature range (PTTR) was measured. The effects of the heating and cooling rates with which the gage passed through the PTTR on the apparent strain characteristics of the gage were also studied. BCL3 gage, like other Fe-Cr-Al based gages, exhibited apparent strain instability in the temperature range of 700 to 1100 F due to the reversible microstructural transition the gage materials experienced in this temperature range. The BCL3 gage had a maximum apparent strain drift in the neighborhood of 770 F with an average drift rate of approx. -440 microstrain/hr in 2 hrs. The use of the BCL3 gage as well as other Fe-Cl-Al based gages for static strain measurements within the PTTR should be avoided unless the time durations in the PTTR are small enough to introduce a neglible drift. The microstructure transition that the BCL3 gage underwent occurred in the temperature range of 750 to 1050 F during heating and around 1000 to 800 F during cooling. The heating rate, and, in particular, the cooling rate with which the gage passed through the PTTR affected the shape and the repeatability of the apparent strain curve of the gage.

Lei, Jih-Fen↗

Development and pilot line production of lithium doped silicon solar cells

Scaling up the BCl3 without O2 diffusion beyond 30 to 40 cells was investigated by using a 100 cell capacity diffusion boat which held the cells vertically. Sheet resistances and I-V curves were uniform with 10 to 20 cells spaced along the entire boat, so the quantity was increased to 40 and then 60 cells per diffusion. There was no change in cell output and uniformity going from 20 to 40 cells per diffusion; however only half the lithium cells fabricated from slices diffused in the 60 cell diffusion had efficiencies of 11% or better. Although uniform sheet resistances and I-V characteristic curves were obtained with up to 60 cells in the BCl3 with O2 diffusion, the short circuit currents were approximately 15% lower than the anticipated 135 to 140 mA. Consequently, work on this diffusion process has been aimed solely at increasing the short circuit current. The diffusion temperature was lowered from 1055 to 1000 and 950 C, and at each of these temperatures variations in diffusion time were investigated. At 1000 C short circuit currents were approximately 10 mA higher, 130 rather than 120 mA average.

Payne, P. A.↗

Development and pilot line production of lithium doped silicon solar cells

The work performed over the period of September 1971 to August 1972 to develop production processes for fabrication of lithium doped P/N cells is described. The BCl3 diffusion without 02 was selected as the optimum diffusion process for fabrication of lithium doped cells. An 8-2-7 (warm up - deposition - drive-in time in minutes) diffusion schedule at 1055 C was used for the first two lots (300 cells each) delivered to JPL. Cell efficiencies ranged from 11.0 to 13.7% based on an AMO of 135.3 mW/sq cm. These high efficiencies were obtained using from 10 to 40 cells per boron diffusion; increasing the quantity beyond 40 resulted in lower outputs. At this point, the emphasis was placed on investigation of a BCl3 with 02 diffusion. Through evaluation of the effects of diffusion time and temperature, gas flow rates, and desposition plus drive-in vs. continuous deposition and no drive-in cycles, diffusion parameters were determined which produced short circuit currents of 136 + or - 4 mA for ten cells spaced along 12 in. of the diffusion boat. The quantity was increased to 60, 100, and 150 cell diffusions with no more variation in cell short circuit current than observed with 10 cells.

Payne, P. A.↗

Development of large diameter carbon monofilament

A process for preparing large diameter carbon-boron monofilament was developed. The process involves chemical vapor depositing a carbon-boron alloy monofilament from a BCl3, CH4, and H2 gas mixture onto a carbon substrate. Amorphous alloys were formed when gaseous mixtures containing greater than 20 percent methane (80 percent BCl3) were used. The longest uninterrupted lengths of carbon-boron monofilament were produced using a CH4/BCl3 gas ratio of 2.34. It was found that the properties of the carbon-boron alloy monofilament improved when the carbon substrate was precleaned in chlorine. The highest strength monofilament was attained when a CH4/BCl3 gas volume ratio of 0.44 was 28 million N/sq cm (40 million psi). While the highest strengths were attained in this run, the 0.44 gas ratio and other CH4/BCl3 ratios less than 2.34 would not yield long runs. Runs using these ratios were usually terminated because of a break in the monofilament within the reactor. It is felt better process control could probably be achieved by varying the amount of hydrogen; the BCl3/H2 ratio was kept constant in these studies.

Jacob, B.↗

A Reactive-Ion Etch for Patterning Piezoelectric Thin Film

Reactive-ion etching (RIE) under conditions described below has been found to be a suitable means for patterning piezoelectric thin films made from such materials as PbZr(1-x)Ti(x)O3 or Ba(x)Sr(1.x)TiO3. In the original application for which this particular RIE process was developed, PbZr(1-x)Ti(x)O3 films 0.5 microns thick are to be sandwiched between Pt electrode layers 0.1 microns thick and Ir electrode layers 0.1 microns thick to form piezoelectric capacitor structures. Such structures are typical of piezoelectric actuators in advanced microelectromechanical systems now under development or planned to be developed in the near future. RIE of PbZr(1-x)Ti(x)O3 is usually considered to involve two major subprocesses: an ion-assisted- etching reaction, and a sputtering subprocess that removes reactive byproducts. RIE is favored over other etching techniques because it offers a potential for a high degree of anisotropy, high-resolution pattern definition, and good process control. However, conventional RIE is not ideal for patterning PbZr(1-x)Ti(x)O3 films at a thickness as great as that in the original intended application. In order to realize the potential benefits mentioned above, it is necessary to optimize process conditions . in particular, the composition of the etching gas and the values of such other process parameters as radio-frequency power, gas pressure, gas-flow rate, and duration of the process. Guidelines for determining optimum conditions can be obtained from experimental determination of etch rates as functions of these parameters. Etch-gas mixtures of BCl3 and Cl2, some also including Ar, have been found to offer a high degree of selectivity as needed for patterning of PbZr(1-x)Ti(x)O3 films on top of Ir electrode layers in thin-film capacitor structures. The selectivity is characterized by a ratio of approx.10:1 (rate of etching PbZr(1-x)Ti(x)O3 divided by rate of etching Ir and IrO(x)). At the time of reporting the information for this article, several experiments on RIE in BCl3 and Cl2 (and sometimes Ar) had demonstrated the 10:1 selectivity ratio, and further experiments to enhance understanding and obtain further guidance for optimizing process conditions were planned.

Yang, Eui-Hyeok↗

Additional development of large diameter carbon monofilament

The chemical vapor process for preparing a large diameter carbon-base monofilament from a BCl3, Ch4 and H2 gas mixture with a carbon substrate fiber was studied. The effect of reactor geometry, total gas flows and deposition temperature on the tensile strength of the monofilament were investigated. It was noted that consistent results could only be obtained when the carbon substrate fiber was cleaned. The strength of the monofilament was found to depend on the highest temperature and the temperature profile of the monofilament in the reactor. The strength of monofilament produced in the dc and RF reactors were found to be similar and similar alloy compositions in the monofilament were attained when the same gas ratios were used. The tensile strength of the monofilament at 500 C was found to be 60 to 70% of the room temperature tensile strength. No degradation was noted after exposure to molten aluminum.

Jacob, B. A.↗

Residual stresses in boron/tungsten and boron/carbon fibers

Longitudinal residual stress distribution is determined for 102-micron diam B/W and B/C fibers. The 102-micron diam B/W fibers are deposited on a 12.7-micron diam tungsten wire resistively heated in a BCl3-H2 reactor. The 102-micron diam B/C fibers are made by deposition of boron on a pyrolytic graphite-coated carbon fiber. The longitudinal residual stress distribution is calculated from measurements of the change in length of the fiber produced by removal of the surface through electropolishing. It is found that for both types of fibers, the residual stress vary from a compressive stress at the surface to a tensile stress in the boron near the core. Closer to the core and in the core, significant differences in the residual stresses are observed for the B/W and B/C fibers.

Behrendt, D. R.↗

Experimental studies of the formation/deposition of sodium sulfate in/from combustion gases

Interference in a reflected beam of monochromatic light from a linearly polarized helium-neon laser was used to determine the dew point and deposition rate of B2O3 on a heated platinum target. Preliminary results at different BCl3 seed levels, except for one flow velocity and equivalence ratio (.813) are presented and discussed. Alkali chloride reactions with atomic oxygen were also investigated. Readily detectable Na*(g) and K*(g) - atoms were observed in emission at 589 nm, 766nm, 796nm, respectively.

Rosner, D. E.↗

Experimental studies of the formation/deposition of sodium sulfate in/from combustion gases

An optical polarization (ellipsometric) technique was developed for measuring rapidly growing and evaporating transparent liquid condensate films (e.g., boric oxide) on solid surfaces exposed to combustion product gases. Results for the B2O3 deposition rate from BCl3-seeded propane/air flames are shown to agree well with the results of earlier interference measurements, and also with theoretical CVD predictions. Evaporation rates (from platinum ribbons into seeded propane air flames) are estimated using the polarization technique. It appears that, compared with the interference method, the polarization technique places less stringent requirements on surface quality, which may justify the added optical components needed for such measurements. It is concluded that the complementary optical methods of polarization (ellipsometry) and interference hold considerable promise for application to the rapid measurement of condensation and evaporation rates in high temperature (e.g., combustion product) environments.

Rosner, D. E.↗

Investigation of etching techniques for superconductive Nb/Al-Al2O3/Nb fabrication processes

Wet etching, CF4 and SF6 reactive ion etching (RIE), RIE/wet hybrid etching, Cl-based RIE, ion milling, and liftoff techniques have been investigated for use in superconductive Nb/Al-Al2O3/Nb fabrication processes. High-quality superconductor-insulator-superconductor (SIS) junctions have been fabricated using a variety of these etching methods; however, each technique offers distinct tradeoffs for a given process an wafer design. In particular, it was shown that SF6 provides an excellent RIE chemistry for low-voltage anisotropic etching of Nb with high selectivity to Al. The SF6 tool has greatly improved the trilevel resist junction insulation process. Excellent repeatability, selectivity with respect to quartz, and submicron resolution make Cl2 + BCl3 + CHCl3 RIE a very attractive process for trilayer patterning.

Lichtenberger, A. W.↗