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Article (Published Version) Article Gas phase synthesis of epitaxial layers of nickel-chlorine boracite on chromium-chlorine boracite SCHMID, Hans, TIPPMANN, Heinz Abstract Layers of Ni boracite were epitaxially grown on Cr-Cl boracite at 900 Deg. At the reaction temperature both substrate and layer had the cubic 43m symmetry whereas at room temperature the layer is ferroelectric (symmetry mm2) and the substrate is still cubic. The layers were produced both by (1) CVT reactions in closed quartz ampules and by 2 variants of a CVD process by using either the reactants BCl3(g) + H2O(g), or B2O3(g) for the formation of the intermediate gaseous (BOCl)3 and the B2O3 hydrates. The reactant NiCl2(g) was obtained by reaction Ni(s) + Cl2(g) = NiCl2(g) at .apprx.1000 Deg inside the reactor. Layer thicknesses of 1-100 mm were achieved. The growth rate was .apprx.1 mm/min. The best substrates were those with smooth, as-grown surfaces; these layers were characterized after cooldown by a pattern of ferroelectric 180 Deg domains with the spontaneous polarization oriented perpendicularly to the surface, an average domain size of 1-10 mm and good contrast (at l = 546 nm) between antiparallel domains placed between crossed polarizers and a retarder. The ferroelectric poling fields were >107 V/m. Reference SCHMID, Hans, TIPPMANN, Heinz. Gas phase synthesis of epitaxial layers of nickel-chlorine boracite on chromium-chlorine boracite. Journal of Crystal Growth, 1979, vol. 46, no. 6, p. 723-742 DOI : 10.1016/0022-0248(79)90220-3 Available at: http://archive-ouverte.unige.ch/unige:33303 Disclaimer: layout of this document may differ from the published version. 1 / 1 Journal of Crystal Growth 46 (1979) 723-742 © North-Holland Publishing Company GAS PHASE SYNTHESIS OF EPITAXIAL LAYERS OF NICKEL-CHLORINE BORACITE ON CHROMIUM-CHLORINE BORACITE Hans SCHMID * and Heinz TIPPMAN Battelle Geneva Research Centre, CII-1227 Carouge-Geneva, Switzerland Received 11 January 1979 Layers of Ni-Cl boracite have been epitaxially grown on Cr-Cl boracite at 900°C. At the reaction temperature both substrate and layer had the cubic 43m symmetry whereas at room temperature the layer is ferroelectric (symmetry mm2) and the substrate is still cubic. The layers have been produced both by (i) CVT reactions in closed quartz ampoules and by (ii) two variants of a CVD process using either the reactants BCl3(g) + H20(g), or 8203(1) + H20(g) for the formation of the intermediate gaseous (BOCDa and the B2O3 hydrates. The reactant NiCl2(g) has been obtained by the reaction Ni(s) + Cl2(g) = NiCl2(g) at about 1000°C inside the reactor. Layer thicknesses from 1 up to 100 txm have been achieved. The growth rate was of the order of 1 ixm/ min. The best substrates were found to be those with smooth, as-grown surfaces; these layers were characterized after cool- down by a pattern of ferroelectric 180° domains with the spontaneous polarization oriented perpendicularly to the surface, an average domain size between 1 and 10 lum and by good contrast (at A. = 546 nm) between antiparallel domains placed between crossed polarizers and a retarder. The ferroelectric poling fields were >10^ V m~^. 1. Introduction This means that at equal switching field strength the switching voltage can in principle be made much 1.1. Motivation smaller in the case of boracites, provided they can be produced in the form of relatively thin layers or Orthorhombic boracites are ferroelectric and are wafers. Such sheets would be interesting, because characterized by the symmetry species [1] applications like light gates, passive display, page 43mFmm2. Hence a jumping of the optical indicatrix composers, etc. can be envisaged [3,5]. Whereas com• of the orthorhombic phase by 90° around the ortho- positions with relatively small birefringence (e.g. rhombic c-axis (which is parallel to the spontaneous Fe I boracite with An25°c = 0.004) can be used in polarization and to the pseudo-ctibic (100) direction) the form of self-supporting single crystalline wafers, can take place upon 180° reversal of the spontaneous compositions with higher An necessitate the fabrica• polarization [2-5]. This can be achieved by applying tion of epitaxial, substrate-supported layers with a a voltage to the electrodes (e.g. transparent Au on Cr thickness of a few microns if a quarter wave device is [3]) deposited on the facets of wafers cut parallel to desired. pseudocubic (100). This behaviour is similar to that The objective of the work described in this paper of Gd2(Mo04)3, which is characterized by species was to demonstrate the practical feasibility of making 42mFmm2 [6,7]. The switchable spontaneous such layers by a chemical process. birefringence at room temperature is about 10—15 times higher in orthorhombic boracites (An: 0.004 1.2. Approach to 0.022) [4] than in Gd2(Mo04)3 (A«: 0.0004). The fabrication of epitaxial boracite layers seemed possible by modifying one of the two previously * Present address: Department of Inorganic, Analytical and Applied Chemistry University of Geneva, 30, quai Ernest known methods of obtaining single crystalline borac• Ansermet, CH-1211 Geneva 4, Switzerland. ite, namely: the hydrothermal or hydrothermal-like 723 724 H. Schmid, H. Tippmann / Gas phase layers of Ni-Cl boracite method [8—18], or the chemical vapour transport Table 1 (CVT) method [19-23]. Potential point groups and crystallographic cuts of substrates The gas phase approach was finally chosen, appropriate for switchable layers of orthorhombic boracite because of easier control of the experimental para• Crystal system Point group Possible cuts meters and because it entails less risk of partial replacement of the halogen by OH than the hydro- Cubic m3m thermal method. Because of the well-known tendency 432 of increase of the Curie temperature in the series I -> 43m m3 (100) Br -> CI F ^ OH boracite, the partial incorporation 23 of OH was expected to lead to an undesirable increase Tetragonal 4 (001) of switching field strength of hydrothermal halogen 42m (001) boracites. 2. Choice of the substrate material oriented paraUely to the surface of the substrate. For the symmetry species 43mFmm2 of the layer it is 2.1. The binary axis condition mandatory that the substrate surface possesses a binary axis perpendicularly to itself. If, on the con• If a layer of orthorhombic boracite is to be used trary, a substrate with a four-fold symmetry axis is for contrast modulation by electric field switching of used, two kinds of crystallite, mutually related by a the orientation of the spontaneous birefringence, that 7t/2 rotation would be obtained with equal probabil• layer has to be single crystalline and in its cubic high ity, and the average transmission between crossed temperature phase with one of the cubic (100) planes polarizers and a retarder would remain identical for Table 2 Estimated data of enthalpy and entropy of formation of some boracites, M3B7O13X (units inkcal mole"* and cal deg"' mole -1 respectively) M X CI Br I •^298 •5298 •5298 A//298 Mg 71.9 -1494 74.7 -1479 76.2 -1460 (Ti)^) 78.0 80.3 83.5 (V) ^) -1361 -1348 -1334 Cr -1297 -1285 -1277 Mn 95.2 -1345 97.9 -1333 99.5 -1317 Fe 91.8 -1258 92.9 -1247 94.5 -1232 Co 84.2 -1239 87.5 -1228 88.9 -1212 Ni 81.2 -1237 82.3 -1226 83.8 -1210 Cu 94.1 -1174 87.2 -1167 88.7 -1150 Zn 84.4 -1315 87.9 -1304 90.5 -1290 Cd 92.1 -1258 93.9 -1249 98.1 -1236 Boracite unknown. Remark: Entropy data obtained by Kelley's "sum method" (see e.g. ref. [38]); the AH° data given in the table are based on the assumption that the enthalpy of formation from the components MO(s), B203(s) and MX2(s) was approximately zero. The real values are probably 5—6% more negative as can be estimated from a comparison of the method applied to Cd and Ca borates [31] of similar metaloxide/B203 ratio as occurring in boracite. The data for the entropies and enthalpies of the components were taken from ref. [42], those of VO(s) fromref. [19] and 5°298 of CrO from ref. [43]. H. Schmid, //. Tippmann / Gas phase layers of Ni-Cl boracite 725 both up and down polarity of the applied field. The Table 3 same is true for a random orientation of crystalHtes Mean cubic lattice parameter misfit of some orthorhombic having (lOO)cub parallel to an isotropic substrate sur• boracites with cubic Cr-Cl boracite at room temperature face, and equally for a poly crystalline ceramic mate• Boracite, mm2 at 20''C Misfit with Cr-Cl boracite rial with prototypic symmetry 43m. (%) 2.2. Tlie thermal expansion condition Mg-Cl -0.42 Mn-Cl 1.33 Mn-Br 1.39 Because the composition of the boracite layer is Mn-I 1.68 cubic at the deposition temperature and remains Fe-1 0.93 cubic for several hundred degrees during cooling, it is Ni-Cl -0.70 necessary that the thermal expansion coefficient of Ni-Br -0.71 the substrate is isotropic in the contact plane. This Cu CI -0.72 Zn-Br -0.30 requirement reduces very much the possibiUties of Zn-I -0.25 choice of the substrate. As shown on table 1, it can Cd CI 3.00 be fulfilled for substrates with one of the five cubic Cd-Br 3.1 point groups or with one of the tetragonal groups 4 Cd-I 3.6 or 42m. The orthorhombic groups mmm and 222 and the Definition of misfit = [ Aa^ub/'^cub^'"®^'^)] ^ ^^O.
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