• Proceedings of the Korea Association of Crystal Growth Conference
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• 1996.06a
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• pp.258-292
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• 1996

In the last year great interest appears to YBCO thin films preparation on different substrate materials. Preparation of epitaxial film is a very difficult problem. There are many requirements to substrate materials that must be fullfilled. Main problems are lattice mismatch (misfit) and similarity of structure. From paper [1] or follows that difference in interatomic distances and angles of substrate and film is mire important problem than similarity of structure. In this work we present interatomic distances and angle relations between substrate materials belonging to ABCO4 group (where A-Sr or Ca, B-rare earth element, C-Al or Ga) of different orientations and YBCO thin films. There are many materials used as substrates for HTsC thin films. ABCO4 group of compounds is characterized by small dielectric constants (it is necessary for microwave applications of HTsC films), absence of twins and small misfit [2]. There most interesting compounds CaNdAlO4, SrLaAlO4 and SrLaGaO4 were investigated. All these compounds are of pseudo-perovskite structure with space group 14/mmm. This structure is very similar to structure of YBCO. SLG substrate has the lowest misfit (0.3%) and dielectric constant. For preparation of then films of substrates of this group of compound plane of <100> orientation are mainly used. Good quality films of <001> orientations are obtained [3]. In this case not only a-a misfit play role, but c-3b misfit is very important too. Sometimes, for preparation of thin films substrates of <001> and <110> orientations were manufactured [3]. Different misfits for different YBCO faces have been analyzed. It has been found that the mismatching factor for (100) face is very similar to that for (001) face so there is possibility of preparation of thin films on both orientations. SrLaAlO4(SLA) and SrLaGaO4(SLG) crystals of general formula ABCO4 have been grown by the Czochralski method. The quality of SLA and SLG crystals strongly depends on axial gradient of temperature and growth and rotation rates. High quality crystals were obtained at axial gradient of temperature near crystal-melt interface lower than 50℃/cm, growth rate 1-3 mm/h and the rotation rate changing from 10-20pm[4]. Strong anisotropy in morphology of SLA and SLG single crystals grown by the Czochralski method is clearly visible. On the basics of our considerations for ABCO4 type of the tetragonal crystals there can appear {001}, {101}, and {110} faces for ionic type model [5]. Morphology of these crystals depend on ionic-covalent character of bonding and crystal growth parameters. Point defects are observed in crystals and they are reflected in color changes (colorless, yellow, green). Point defects are detected in directions perpendicular to oxide planes and are connected with instability of oxygen position in lattice. To investigate facets formations crystals were doped with Cr3+, Er3+, Pr3+, Ba2+. Chromium greater size ion which is substituted for Al3+ clearly induces faceting. There appear easy {110} faces and SLA crystals crack even then the amount of Cr is below 0.3at.% SLG single crystals are not so sensitive to the content of chromium ions. It was also found that if {110} face appears at the beginning of growth process the crystal changes its color on the plane {110} but it happens only on the shoulder part. The projection of {110} face has a great amount of oxygen positions which can be easy defected. Pure and doped SLA and SLG crystals measured by EPR in the<110> direction show more intensive lines than in other directions which allows to suggest that the amount of oxygen defects on the {110} plane is higher. In order to find the origin of colors and their relation with the crystal stability, a set of SLA and SLG crystals were investigated using optical spectroscopy. The colored samples exhibit an absorption band stretching from the UV absorption edge of the crystal, from about 240 nm to about 550 m. In the case of colorless sample, the absorption spectrum consists of a relatively weak band in the UV region. The spectral position and intensities of absorption bands of SLA are typical for imperfection similar to color centers which may be created in most of oxide crystals by UV and X-radiation. It is pointed out that crystal growth process of polycomponent oxide crystals by Czochralski method depends on the preparation of melt and its stoichiometry, orientation of seed, gradient of temperature at crystal-melt interface, parameters of growth (rotation and pulling rate) and control of red-ox atmosphere during seeding and growth (rotation and pulling rate) and control of red-ox atmosphere during seeding and growth. Growth parameters have an influence on the morphology of crystal-melt interface, type and concentration of defects.

• Progress in Superconductivity
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• v.7 no.2
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• pp.140-144
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• 2006

We fabricated the YBCO films on single crystal $LaAlO_3$ substrates via a metal organic deposition (MOD) process. In the process, $Y_2Ba_1Cu_1O_x$ and $Ba_3Cu_5O_8$ powders were dissolved in trifluoroacetic acid (TFA) followed by calcining and firing heat treatments. To evaluate the effects of the firing temperature on YBCO phase formation and critical properties, the films were fired at $750^{\circ}C,\;775^{\circ}C\;and\;800^{\circ}C$ after calcining at $430^{\cric}C$. Microstructure observation indicated that a crack-free surface formed and a strong biaxial texture was developed. The FWHM of out-of-plane texture was measured to be in the range of $4.3^{\cric}-7.0^{\circ}$ for all the films. When the YBCO film was fired at $775^{\cric}C$, it had the highest critical properties: 88.5 K of critical temperature and 16 A/cm-width of critical current ($1MA/cm^2$ as critical current density). On the other hand, those properties were degraded as firing at $750^{\circ}C\;and\;800^{\circ}C$. It is considered that the improved critical values are partly owing to dense and homogeneous microstructure, strong texture, and high oxygen content.

• Progress in Superconductivity
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• v.9 no.1
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• pp.96-101
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• 2007

[ $YBa_2Cu_3O_{7-{\delta}}$ ] films have been prepared on $LaAlO_3$ (100) single-crystal substrates by a metalorganic deposition using dichloroacetate precursors (DCA-MOD). Calcination conditions were varied in order to optimize the microstructure and the superconducting properties of YBCO film. Coated films were calcined at various temperatures ranging from $400{\sim}700^{\circ}C$ in flowing humid oxygen atmosphere. Ramping rate to calcination tempertures was $2.22^{\circ}C/min$. Conversion heat treatment was performed at $800^{\circ}C$ for 2 h in flowing Ar gas containing 1000 ppm oxygen with a humidity of 9.45%. Observations of surface and cross sectional SEM microstructure showed that the particle size in the calcined film increased in the range of 100-200 nm with heating rate and the calcination temperature. SEM EDS analysis showed that 13 a/o of chlorine was contained in the calcined film. It was also observed that the porosity increased with the heating rate and temperature. Porous microstructure was developed when YBCO films were prepared using porous calcined film. Dense microstructure and high $J_c$ over $1\;MA/cm^2$ was obtained when calcination was carried out at the temperature of $500^{\circ}C$ with a heating rate of $2.22^{\circ}C/min$.

• Progress in Superconductivity
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• v.9 no.1
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• pp.102-106
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• 2007

YBCO films have been synthesized using a spray pyrolysis method. We used nitrates of Y, Ba, Cu as precursors. Deposition was made on $LaAlO_3$ (100) single crystal substrate by spraying the mist of aqueous precursor solution generated by a concentric nozzle. The distance between concentric nozzle and substrate was 15 cm. C-axis oriented films were obtained at deposition temperature of $740{\sim}800^{\circ}C$ and working pressure of 20 Torr. Oxygen partial pressure was 3 Torr and substrate was transported with the speed ranging from 0.23 cm/min to 0.7 cm/min by reel to reel. Scanning electron microscope (SEM) and X-ray diffraction (XRD) observation revealed that films are smooth and highly textured with (001) planes parallel to substrate. Highest critical current density (Jc) was $1.38\;MA/cm^2$ at 77K and self-field for the film with a thickness of $0.5\;{\mu}m$ prepared at a substrate temperature of $780^{\circ}C$ and $PO_2\;=3\;Torr$. The effect of temperature on the microstructure and YBCO phase formation will be discussed.

• Progress in Superconductivity
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• v.8 no.1
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• pp.71-74
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• 2006

High $J_c$ over 1 $MA/cm^2$ YBCO film has been successfully prepared using nitrate precursors by spray pyrolysis method. Aerosol drolpets generated using a concentric spray nozzle were directly sprayed on a $LaAlO_3$(100) single crystal substrate. The cation ratio of precursor solution was Y:Ba:Cu=1:2.65:1.35. The distance between nozzle and substrate was 15 cm. Deposition temperature was ranging from $750^{\circ}C\;to\;800^{\circ}C$. Deposition pressure was 100 Torr, and oxygen partial pressure was varied from 10 Torr to 50 Torr. The microstructure, phase formation, texture development and superconducting properties of deposited films were largely changed with oxygen partial pressure. Deposited films showed a texture with(001) planes parallel to substrate plane. High quality film was obtained when film was deposited at $760^{\circ}C$ with an oxygen partial pressure of 30 Torr. The critical current density($J_c$) of the YBCO film was 1.75 $MA/cm^2$ at 77 K and self-field.

• Progress in Superconductivity
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• v.8 no.1
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• pp.93-97
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• 2006

YBCO films were deposited on a moving substrate by a spray pyrolysis method using nitrate aqueous solution as precursors. Deposition was made on $LaAlO_3$(100) single crystal substrate by spraying precursor droplets generated by a concentric nozzle. The cation ratio of precursor solution was Y:Ba:Cu=1:2.65:4.5. The distance between nozzle and substrate was 15 cm. Substrate was transported with a speed ranging from 0.23 cm/min to 0.5 cm/min. Films were deposited at the pressure ranging from 10 Torr to 20 Torr and the deposition temperature was ranged from $740^{\circ}C\;to\;790^{\circ}C$. Oxygen partial pressure was controlled between 1 Tow and S Torr. Superconducting YBCO films were obtained from $740^{\circ}C\;to\;790^{\circ}C$ with an oxygen partial pressure of 3 Torr. Scanning electron microscope(SEM) and X-ray diffraction(XRD) observation revealed that films are smooth and highly texture with(001) plans parallel to substrate plane. Highest Jc was 0.72 $MA/cm^2$ at 77K and self-field for the film with a thickness of 0.15 m prepared at a substrate temperature of $740^{\circ}C$ and $PO_2$=3 Torr.

• Progress in Superconductivity
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• v.8 no.1
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• pp.59-64
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• 2006

High $J_c\;YBa_2Cu_3O_x$ superconducting films were fabricated by MOD method using fluorine-free dichloroacetic acid(DCA) as chelating solvent for preparing precursor solution. Coating solutions were prepared by dissolving Y-, Ba- and Cu-acetates in DCA solvent followed by drying in rota vapor to obtain the blue gel that is diluted in methanol and 2-methoxyethanol for adjusting the cation concentration. DCA-MOD precursor solution was coated on a single crystal(001) $LaAlO_3(LAO)$ substrate by a dip coating method with a speed of 25 mm/min. Coated films were calcined at lower temperature up to $500^{\circ}C$ in flowing oxygen atmosphere with a 7.2% humidity. Conversion heat treatment was performed at various temperatures of $780{\sim}810^{\circ}C$ for 2 h in flowing Ar gas containing 1000 ppm oxygen with a humidity of 9.45%. SEM observations showed that films have very dense microstructures for the films prepared at the temperature higher than $800^{\circ}C$ regardless of diluting solvent; methanol or 2-methoxyethanol. X-ray diffraction analysis showed that YBCO grains grew with a (001) preferred orientation. A High critical current density($J_c$) of 1.28 $MA/cm^2$(@77 K and self-field) was obtained id. the YBCO film prepared using 2-methoxyethanol as a solvent.

• Proceedings of the KIEE Conference
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• 2005.07c
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• pp.2001-2003
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• 2005

Various organic acid were used in order to prepare new metalorganic deposition solution for high quality $REBa_2Cu_3O_{7-{\delta}}$ (RE=Y, Eu, Gd) films. Prepared fluorine free MO precursor solution was coated on single crystal (001) $LaAlO_3$ (LAO) by dip coating method. Processing parameters such as oxygen partial pressure, water vapor, ramping rate and pyrolysis temperature etc havebeen controlled in order to make high $J_c$ films with a good epitaxial relationship with substrate. 0.5 micron-thick film was obtained by single coating and no crack appeared after calcination. Oxygen partial pressure was varied in the range of $100{\sim}1,000 ppm$ and conversion heat treatment was carried out at the temperature of $725{\sim}765^{\circ}C$. A critical transition temperature $(T_{c0})$ of 90K and a critical transport current density $(J_c)$ of $>0.5MA/cm^2$ (77K and self-field) were demonstrated for the YBCO film on (001) oriented LAO substrates with a thickness of 0.5 micron. $I_c$ was determined by utilizing a transport measurement. SEM and XRD investigations confirmed that films were grown epitaxially onto the LAO single crystal substrate. It is thought that fluorine free new MOD solutionis promising for high quality REBCO films.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1998.06a
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• pp.367-370
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• 1998

In this paper, based on the research of high temperature YBCO superconductor, using the Yb instead of Y, with the YbBCO superconductor powder which was combined by means of conventional solid reaction, textured directional crystal was prepared by MCP method and the character was analyzed. Mixing the starting elements and calcining at 890$^{\circ}C$, 900$^{\circ}C$, 910$^{\circ}C$, single phase YbBCO, Yb$_2$BaCuO$\sub$5/ and BaCuO$\sub$2/ were certified. And from the powder which was calcined at 900$^{\circ}C$ the, sample which became texture-growth by MCP method was well oriented. The result of DTA measurement, the fusing point of YbBCO superconductor and it\`s critical current was measured to be 979$^{\circ}C$, 87K respectively. The critical current density was obtained at the value of 700A/$\textrm{cm}^2$(77K. 0H) calculated by Bean's Model using the measured hysteresis curve of VSM.

• Progress in Superconductivity and Cryogenics
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• v.20 no.3
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• pp.5-10
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• 2018

This study presents that various grain boundary junctions are prepared by controlling the seed orientation combined with an artificial hole in a melt process REBCO bulk superconductor. Large grain YBCO superconductors have been fabricated with various grain boundary junctions that the angle between the grain boundary and the <001> axis of Y123 crystal is $0^{\circ}$, $30^{\circ}$ and $45^{\circ}$, respectively. The presence of the artificial hole is beneficial for the formation of clean grain boundary junction and single peak trapped magnetic field profiles have been obtained. Artificial hole makes two growth fronts meet at a point on a periphery of the artificial hole. The presence of artificial hole is not likely to affect on the distribution of Y211 particles. The newly formed <110> facet lines are explained by the formation of new Y123/liquid interface with (010) crystallographic plane.