METHOD FOR MANUFACTURING OXIDE POWDER HAVING PEROVSKITE STRUCTURE AND OXIDE POWDER MANUFACTURED BY SAME

Hereinafter, with reference to the drawing objects of the present invention in the embodiment detailed with respect to each other. The present invention refers to various modification may have bar can apply in various forms, in the embodiment herein detailed drawing and example are specific to broadcast receiver. However this particular disclosure be but is defined with respect to the present invention form, all changing range of idea and techniques of the present invention, including the water to replacement should understood to evenly. Each drawing are described as well as a component while similar references in a similar.

The application specific term used in the present invention is only intending to be used to account for in the embodiment defining is endured. It is apparent that a single representation of the differently in order not providing language translators, comprising plurality of representation. In the application, the term "comprising" or "having disclosed" specification of articles feature, step, operation, component, piece or specify a combination not present included, another aspect of one or more moveable step, operation, component, piece or a combination of pre-times the number should not understood to presence or additional possibility.

Not defined differently, scientific or technical terms so that all terms in the present invention thus is provided to the person with skill in the art will generally have the meanings etc. by same. Dictionary used for such as generally defined on the context of respective technical terms have the meanings must be consistent semantics and having interprets, the application will not become manifest in defining, or overly formal sense interpreted not ideal.

Figure 1 shows a method of the present invention having a perovskite structure oxide powders in a number one in the embodiment according to also describe sequences for tank are disclosed.

1 Also reference surface, at least one of a metallic ingredient including at least 3, having a perovskite structure oxide powder EDTA (ethylenediaminetetraacetic acid) solution and high pressure liquid coolant metal precursor solutions in order number (EDTA-a NH₃ ) Is prepared and each mixing chamber.

Said at least 3 species of different metal precursor and ethanol (ethanol, ethyl alcohol) metal precursor solutions by mixing 4700. Ethanol said metal precursors to disperse said metal precursors to form a metallic ion ionized simultaneously formed on the substrate. Metal ions from the distilled water collecting as a solvent (sol) forming a sol gel (gel) in mode switch is used in the process to the first and the second evaporation time distilled gelling by subjecting removed in strong-with each other. the metal precursor are ethanol thereby dispersing the door number can be solve. Said metal precursor solutions may also include lanthanide metal precursor, barium (Ba) precursor, copper (Cu) (Co) precursor and precursor comprises cobalt. The, lanthanide metal precursor contained in the lanthanide metal uses, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Lu or a Yn is cited. In particular, lanthanide metal as, Pr, Nd, Pm, Sm, Eu or Gd can be using, preferably Pr, can be using Nd or Gd.

Said lanthanide metal precursor, barium (Ba) precursor, and copper (Cu) precursor cobalt (Co) precursor and, by using the same LnBaCo_{(2 Non-x)} Cu_x O_{5 + Δ} Form (0<x<2, represents Ln comprises lanthanum group metals) 4 component oxide having a perovskite structure of number can be high pressure liquid coolant. The, depending on the organic comprises a mixing x bark content can be. Said perovskite structure be a layered perovskite structure.

Said EDTA solution (EDTA-a NH₃ ) Weight (NH₄ OH) can be prepared by mixing a adding EDTA.

Said metal precursor solution prepared as in said EDTA solution (EDTA-a NH₃ ) Mixing a liquid sol (sol) similar liquid phase with each other. Adding citric acid (citric acid) having similar liquid sol mixture can be referred to as the sol (sol) is passed into the substantially and, in this state continuously agitate gelling to gel (gel) formed on the substrate. Sol having similar liquid mixture mixed with citric acid, then stirring until transparent or translucent sol (clean sol), stirring continuously extrudes gel (gel) can be formed. Said process of forming and sol sol (sol) (sol) can be carried out in each of the 50 to 70 °C a gelling temperature condition.

In a process of gelling, chuck including metal precursor solution is combined with a low number of chelating a chelate reaction in EDTA is citric acid on metal cation between agglomeration has taken place, this agglomeration due to aggregation in the rear but far after crystallized powders, in the present invention number when said high pressure liquid coolant metal precursor solution by using ethanol to minimize agglomeration can be crystallized in addition between minimizing agglomeration of powders can be.

Citric acid sol (sol) pH 9 to 10 by mixing preferably in forming conditions. PH 9 to 10 said conditions when performing the test, a compound having a structure other than perovskite structure is formed but additional door number, if pH 9 to 10 is carried out in a range having a perovskite structure oxide powder formed therein.

Then, 200 to 300 °C (solid oxide powders in a precursor) in gel is dried to solid product can be obtained.

Calcining said solid product at a temperature of at least 450 °C so that, oxide powder can be formed. The metal oxide particles are formed in the crystallized solid product calcination process by metal oxide powder formed therein. The calcination process implementation being 1,000 °C to 450 °C temperature condition. From the distilled water collecting metal precursor solution at least 1,000 °C exceeds the mode switch is used under temperature conditions of a calcination process but, by using distilled water instead of ethanol by metal oxide powder can be 1,000 °C to 450 °C in calcined form. Most preferably, in 950 °C calcination to form metal oxide powder.

Said process described manufacturing method of the existing method number along a powder prepared by the perovskite structure by sol - powder having a perovskite structure have an perovskite structure when compared to simultaneously exhibits significantly high dispersibility-surface properties. In addition, layered perovskite structure can be formed highly powder is dispersed stably. Having perovskite structure powder is mixed ionic and mixing these properties has electric conductivity, solid oxide cell conductive oxide electrode consisting of solid oxide cell deterioration of can be improve characteristic.

In the embodiment 1: oxide powder sample 1 number of bath

Praseodymium (Pr) precursor, barium (Ba) precursor, copper (Cu) cobalt (Co) precursor and the oxide component PrBaCo 4 using precursors_{1. 9} Cu_{0. 1} O_{5 + Δ} In order to form high pressure liquid coolant after weighing into a stoichiometric excess of number, these ethanol after dissolving magnetic bars are agitated by precursor solution Royal (stir). The, praseodymium precursor include Pr (NO₃ )₂ , 6H₂ Using O have, barium precursor, cobalt precursor and bark each as Ba (NO₃ )₂ , Co (NO₃ )₃ , 6H₂ O, Cu (NO₃ )₂ , 2. 5H₂ O using a transparent conductive layer, each of 1:1:19:0. 1 Molar ratio is mixed.

Then, a deionized water is mixed with a high pressure liquid coolant number EDTA solution, prepare the precursor solution have in said mixing, citric acid (citric acid) mixed solution (sol) in same agitating mixing 60 °C sol was prepared. The, when the pH is adjusted to pH 9 using ammonia, praseodymium ion, barium ion, cobalt ion and copper ion silica based on the total metal, the molar ratio of 1:1:1 EDTA and citric acid (citric acid)5 Is set to.

Then, in sol gel (gel) to 60 °C (maintaining pH 9) are agitated [...] continues until, at the time when the gel dried 250 °C after solid product obtained. Calcining said solid product was obtained in a high pressure liquid coolant sample number 1 450 °C oxide powder.

In the embodiment 2: number of sample 2 bath

By the same process as in the embodiment 1 according to the bath for a sample number 1, number 2 was carried out in a high pressure liquid coolant according to a calcination process 950 °C sample of the present invention in the embodiment 2.

Comparison 1 and 2: number of comparison sample 1 and 2 bath

Praseodymium precursor, barium precursor, a cobalt precursor and seed [...] bark ethanol distilled water instead of the number and, in the embodiment 1 according to a number of annealing bath sample 1 sample 1 was substantially the same high pressure liquid coolant through a number comparison process.

In addition, praseodymium precursor, barium precursor, a cobalt precursor and seed and bark ethanol distilled water instead of the number [...], sample 2 in the embodiment 2 according to a number of annealing process through a high pressure liquid coolant bath substantially the same comparison sample 2 his number.

Structural analysis: TEM analysis

Said prepared sample in 1, 2, 1 and 2 comparison sample was photographed in TEM relative to each other. Also exhibits 2 and 3 also to result.

Figure 2 shows a sample prepared by the number of the present invention in the embodiment 1 according to example 1 of the sample also compared according to transmission electron microscope (TEM) indicating the pictures and comparison prepared by the number drawing, Figure 3 of the present invention in the embodiment 2 according to the example 2 sample prepared by the number indicating the number of samples compared according to TEM pictures comparison produced therewith are disclosed.

In Figure 2 (a) and (b) of sample 1 and compared, (c) and (d) of Figure 2 there has the sample 1, in Figure 3 (a) and (b) of sample 2 and compared, (c) and (d) of Figure 3 of the sample 2 are disclosed.

2 And 3 also the reference also, (c) and (d) of Figure 2 (a) and (b) lower than that in the case of powder without agglomeration which is made up of fine particle formed of Figure 3 (a) and (b) can be confirmed (c) and (d) as compared to the case of making sure that the powder agglomeration can be free. I.e., in the case of comparison sample 1 and 2 using distilled water as a solvent such as in Figure 2 constituting severe powder agglomeration between particles while the, sample 1 and 2 if the edible powder of fine particles in the case of a photograph can be directly compared with conventional TEM order to become usable information. I.e., conductive agglomeration can be confirmed. In Figure 3 (a) and (b) is in particular in the case of, in calcined 450 °C W hen used in generating flocculation due to particle growth by confirming the 950 °C equal to or can be connected to a, (c) and (d) in the case of about 50 nm is generated by the chemical formula 2 relatively uniformly sized particles having a particle growth by choosing a degree can be sure that are distributed.

XRD analysis -1

Example 2 compared to the sample prepared by the number 2 in the embodiment 2 in said sample number 2 according according to XRD analysis for each conducting comparison produced therewith. The result 4 also exhibits.

Figure 4 of the present invention in the embodiment 2 according to example 2 of the sample prepared by the sample number number X - ray diffraction (XRD) analysis compared according to graph comparison produced therewith are disclosed.

In Figure 4, represents diffraction angle axes x, y axes in light intensity (intensity) exhibit a corresponding translucent, compared to sample 2 and lower graph of Figure 4, the upper graph is a sample 2 are disclosed.

The reference also 4, comparison sample 2 and sample 2 strong diffraction peaks at each intensity in the vicinity of translucent 35° 30° to both molecules can be seen. I.e., solvent when using a layered perovskite structure when using ethanol or both PrBaCo chuck_{1. 9} Cu_{0. 1} O_{5 + Δ} Molecules can be formed. In particular, in the case of sample 2 as compared to the comparison sample 2 strong diffraction peaks can be seen significantly intensity molecules.

In the embodiment 3 to 6: number of sample 3 to 6 bath

Process for preparing a controlled pH 7, 8, 10 and 11 using ammonia in number to the number and each [...], number of sample 2 of the present invention in the embodiment 2 according to the first air gap to a high pressure liquid coolant sample number 6 was substantially the same tub 3.

XRD analysis -2

Sample 2 to sample 6 relative to each other, conducting XRD analysis. 5 Exhibits also to result.

Figure 5 shows a tank according to the present invention also according to explain the change in acidity number oxide powder XRD analysis graph representing change product comprising the step of surface are disclosed.

In Figure 5, which is requested to 3 (a), (b) and (c) 4 which is requested to sample 5, which is requested to 2 (d), (e) is requested to 6 are disclosed.

The reference also 5, such as in Figure 4 (a) to (e) both strong diffraction peak intensity in the vicinity of translucent 30° to 35° molecules can be seen. However, of Figure 5 (a), (b) and (e) in the case of a layered perovskite structure is formed but, additionally 2 [...] (second phase) can be formed than that. I.e., of Figure 5 (a), (b) and (c) and (d) and (e) in the case of a new peak appears more exhibited diffraction peaks of the intensity of the diffraction peaks to 35° appears to be relatively weak or 30° can be confirmed. Thus, even when using ethanol as solvent, without concomitant created, layered perovskite structure PrBaCo_{1. 8} Cu_{0. 2} O_{5 + Δ} The most preferred pH range is 9 to 10 in can be confirmed.

Polarization resistance characteristic evaluation

Prepared in example 2 of the present invention in the embodiment 2 according to said sample prepared by the number 2 in comparison with sample 2 relative to each other in polarization resistance characteristic with respect to comparison prepared by the number according to 750 °C was assessed. 6 Also exhibits to result.

Figure 6 of the present invention in the embodiment 2 according to the example 2 sample prepared by the number indicating the number of polarization resistance characteristic with respect to the compared sample comparison produced therewith are disclosed graph.

In Figure 6, and "■ethanol" for sample 2, compared to sample 2 "●water" are disclosed.

6 Also reference surface, using ethanol as solvent distilled water resistance of a comparison sample 2 sample 2 using the cetane number having a value making sure that the resistance can be compared. I.e., comparison sample 2 sample 2 compared to about 25% lower resistance value can be confirmed. These results indicate that, compared to the dispersion of 2 high dispersion of comparison sample 2 sample appears to be according to specific surface can be forced by them. I.e., ethanol can be used when a high pressure liquid coolant number 2, number 2 sample compared using a high pressure liquid coolant from the distilled water collecting when dispersibility can be improved further as compared to directly identify.

In a of the present invention preferred embodiment said through a browser but, if a corresponding splicing one skilled art poriae patent idea of the present invention within a range that the present invention not and area away from may be understand various modifying and changing it will rain.