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We have constructed a high-resolution synchrotron-radiation angle-resolved photoemission (ARPES) spectrometer combined with a combinatorial laser molecular-beam epitaxy (laser MBE) thin film growth system in order to investigate the electronic structure of transition metal oxide thin films. An ARPES spectrometer GAMMADATA SCIENTA SES-100 was selected for the high-throughput and high-energy and angular-resolution ARPES measurements. A total energy resolution of 6.3 meV and a momentum (an angular) resolution of 0.02 Å−1 (0.2°) were obtained at a photon energy of 40 eV. The system is installed at the high-resolution vacuum-ultraviolet beamline BL-1C or the soft-x-ray undulator beamline BL-2C at the Photon Factory as an end-station. Another distinctive feature of this system is the direct connection from the spectrometer to a laser MBE chamber. Thin film samples can be transferred quickly into the photoemission chamber without breaking ultrahigh vacuum. Laser MBE is one of the best methods to grow thin films of many different transition metal oxides and to achieve well-ordered surfaces, which are indispensable for the ARPES measurements. The capabilities of the system and the importance of the in situ sample transfer between ARPES and laser MBE are demonstrated by studying the band structure of La0.6Sr0.4MnO3 thin films epitaxially grown on SrTiO3 substrates by laser MBE.

We have mapped the growth mode of homoepitaxial SrTiO3 thin films as a function of deposition rate and substrate temperature during pulsed laser deposition. The transition from layer by layer growth to step flow growth was mapped by making 260 depositions, 3 monolayers each, on a single substrate. The growth mode was determined by time-resolved reflection high-energy electron diffraction. An atomically smooth surface was regenerated after each deposition by annealing the sample at temperatures above 1200 °C. The depositions were performed at an oxygen pressure of 10−6 Torr and covered a temperature range from 900 to 1380 °C. The effective activation energies of surface migration on Ti- and Sr-terminated surfaces were determined from the mapping results.

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A high-temperature, oxygen compatible, and compact laser molecular beam epitaxy (laser MBE) system has been developed. The 1.06 μm infrared light from a continuous wave neodymium-doped yttrium aluminum garnet (Nd:YAG) laser was used to achieve a wide range and rapid control of substrate temperature in ultrahigh vacuum and at up to 1 atm oxygen pressure. The maximum usable temperature was limited to 1453 °C by the melting point of the nickel sample holder. To our knowledge, this is the highest temperature reported for pulsed laser deposition of oxide films. The efficient laser heating combined with temperature monitoring by a pyrometer and feedback control of the Nd:YAG laser power by a personal computer made it possible to regulate the substrate temperature accurately and to achieve high sample heating and cooling rates. The oxygen pressure and ablation laser triggering were also controlled by the computer. The accurate growth parameter control was combined with real-time in situ surface structure monitoring by reflection high energy electron diffraction to investigate oxide thin film growth in detail over a wide range of temperatures, oxygen partial pressures, and deposition rates. We have demonstrated the performance of this system by the fabrication of homoepitaxial SrTiO3 films as well as heteroepitaxial Sr2RuO4, and SrRuO3 films on SrTiO3 substrates at temperatures of up to 1300 °C. This temperature was high enough to change the film growth mode from layer by layer to step flow.

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