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KR-20260066724-A - Niobic acid compound dispersion and method for preparing the same

KR20260066724AKR 20260066724 AKR20260066724 AKR 20260066724AKR-20260066724-A

Abstract

The niobic acid compound dispersion of the present invention contains niobium, one or more elements X selected from the group consisting of alkali metal elements and alkaline earth metal elements, and a phosphorus compound and/or a chlorine compound, and has a particle diameter (D50) of 1000 nm or less according to dynamic light scattering. In addition, the niobic acid compound dispersion of the present invention contains niobium, one or more elements X selected from the group consisting of alkali metal elements and/or alkaline earth metal elements, and a phosphorus compound and/or a chlorine compound, and has a maximum transmittance of 70%T or more in the wavelength range of 400 nm to 760 nm.

Inventors

  • 미우라 다카시
  • 모토노 류지
  • 하라 슈헤이

Assignees

  • 미쓰이킨조쿠주식회사

Dates

Publication Date
20260512
Application Date
20240903
Priority Date
20230908

Claims (20)

  1. As a dispersion of a niobic acid compound containing niobium, One or more elements X selected from the group consisting of alkali metal elements and alkaline earth metal elements, and It contains one or more compounds selected from the group consisting of phosphorus compounds and chlorine compounds, and A niobic acid compound dispersion characterized by the particle diameter (D50) of the particles in the above niobic acid compound dispersion being 1000 nm or less by dynamic light scattering method.
  2. As a dispersion of a niobic acid compound containing niobium, One or more elements X selected from the group consisting of alkali metal elements and alkaline earth metal elements, and It contains one or more compounds selected from the group consisting of phosphorus compounds and chlorine compounds, and A dispersion of a niobic acid compound characterized by a maximum transmittance of 70%T or more in the wavelength range of 400nm to 760nm.
  3. In Article 1 or Article 2, A niobic acid compound dispersion characterized in that the above element X contains Li.
  4. In Article 1 or Article 2, A niobic acid compound dispersion characterized in that the above-mentioned phosphorus compound contains one or more selected from inorganic phosphorus compounds, organic phosphorus compounds, and salts thereof.
  5. In Paragraph 3, A niobic acid compound dispersion characterized by containing one or more compounds selected from condensed phosphoric acid, pyrophosphate, polyphosphoric acid, phosphoric acid, hypophosphoric acid, ammonium phosphate, ammonium monophosphate, ammonium diphosphate, ammonium pyrophosphate, and ammonium polyphosphate.
  6. In Article 1 or Article 2, A niobic acid compound dispersion characterized by additionally containing one or more compounds selected from the group consisting of ammonia and organic nitrogen compounds.
  7. In Article 1 or Article 2, A niobic acid compound dispersion characterized by having a niobium content of 0.01 mass% or more and 30 mass% or less in terms of Nb atoms.
  8. In Article 1 or Article 2, A niobic acid compound dispersion characterized by having a phosphorus content of 0.01 mass% or more and 10 mass% or less in terms of P atoms.
  9. In Article 1 or Article 2, A niobic acid compound dispersion characterized in that the total amount (M) of element X and the molar ratio M/Nb of niobium (Nb) in the niobic acid compound dispersion is 0.01 or more and 10 or less.
  10. In Article 1 or Article 2, A niobic acid compound dispersion characterized in that the element X in the above niobic acid compound dispersion is Li, and the molar ratio of lithium (Li) to niobium (Nb), Li/Nb, is 0.01 or more and 10 or less.
  11. In Article 1 or Article 2, A niobic acid compound dispersion characterized in that the molar ratio M/(P+Cl) of the total amount (M) of element X in the niobic acid compound dispersion and the total amount (P+Cl) of one or more compounds selected from the group consisting of the phosphorus compound and the chlorine compound is 0.01 or more and 10 or less.
  12. In Article 1 or Article 2, A niobic acid compound dispersion characterized in that the element X in the niobic acid compound dispersion is Li, and the molar ratio Li/(P+Cl) of the total amount (P+Cl) of one or more compounds selected from the group consisting of lithium (Li), the phosphorus compound, and the chlorine compound is 0.01 or more and 10 or less.
  13. In Article 1 or Article 2, A niobic acid compound dispersion characterized in that the molar ratio Nb/(P+Cl) of the total amount (P+Cl) of one or more compounds selected from the group consisting of niobium (Nb), the phosphorus compound, and the chlorine compound in the niobic acid compound dispersion is 0.01 or more and 10 or less.
  14. In Article 1 or Article 2, A niobic acid compound dispersion characterized in that the above-mentioned niobic acid compound dispersion is a water dispersion.
  15. In Article 1 or Article 2, A niobic acid compound dispersion characterized by the particle diameter (D50) of the particles in the above niobic acid compound dispersion being 100 nm or less by dynamic light scattering method.
  16. In Article 1 or Article 2, A niobic acid compound dispersion characterized by having a pH of 2 or higher and 11 or lower.
  17. A niobic acid compound powder characterized by containing a niobic acid compound in a dispersion of the niobic acid compound described in claim 1 or claim 2.
  18. A niobic acid compound film characterized by containing a niobic acid compound in a niobic acid compound dispersion described in claim 1 or claim 2.
  19. A coating agent characterized by containing a dispersion of a niobic acid compound described in claim 1 or claim 2.
  20. A coating agent characterized by containing the niobic acid compound powder described in claim 17.

Description

Niobic acid compound dispersion and method for preparing the same The present invention relates to a dispersion of a niobic acid compound and a method for preparing the same. Lithium niobate, a niobate compound, is utilized as a single crystal in the form of nonlinear optical materials, piezoelectric materials, and battery materials. For example, lithium niobate can be cited as a lithium ion conductive oxide that covers at least a portion of the surface of a composite active material particle capable of reducing the battery resistance generated in an all-solid-state lithium-ion battery. Furthermore, Patent Document 1 discloses a piezoelectric sensor in which a piezoelectric film layer containing lithium niobate powder is formed on a substrate layer of the piezoelectric sensor. In Patent Document 1, the piezoelectric film layer was formed by spray-coating a mixture of lithium niobate powder and a sol-gel solution, and then sintering. FIG. 1 is a table of physical properties of niobic acid compound dispersions according to Examples 1 to 10 and Comparative Examples 1 to 3 of the present invention. FIG. 2 is a table of measurement results of niobic acid compound dispersions according to Examples 1 to 10 and Comparative Examples 1 to 3 of the present invention. Hereinafter, a dispersion of a niobic acid compound according to an embodiment of the present invention will be further explained by the following examples. However, the following examples do not limit the present invention. (Example 1) 0.3g of pyrophosphoric acid (manufactured by Fujifilm Wako Junyaku Co., Ltd., Product Name: Diphosphoric acid (containing phosphoric acid), CAS No.: 2466-09-3) and 28.5g of pure water were placed in a polypropylene container, and 0.84g of a 5 mass% aqueous solution of lithium hydroxide monohydrate was added to the obtained aqueous solution of phosphorus compounds to obtain a mixed solution of phosphorus compounds. Here, a 5 mass% aqueous solution of lithium hydroxide monohydrate was obtained by mixing 15g of LiOH· H₂O with 285g of pure water. Then, 2.93 g of the aqueous solution for neutralizing the niobium compound described below was added to the phosphorus compound mixed solution and stirred for 30 minutes to mix, thereby obtaining a niobic acid compound dispersion according to Example 1. Here, the aqueous solution for neutralizing the niobium compound according to Example 1 was obtained as follows. 100 g of niobium pentoxide was dissolved in 200 g of a 55% aqueous hydrofluoric acid solution, and 830 mL of pure water was added to obtain an aqueous niobium fluoride solution containing 100 g/L of niobium ( Nb₂O₅ = 8.85 mass%) in terms of Nb₂O₅ . 200 mL of this aqueous niobium fluoride solution was added to 1 L of ammonia water ( NH₃ concentration 25 mass%) for less than 1 minute ( NH₃ / Nb₂O₅ molar ratio = 176.9, NH₃ /HF molar ratio = 12.1) to obtain a reaction solution (pH 11). This reaction solution was a slurry of niobic acid compound hydrate, in other words, a slurry of niobium-containing precipitates. Next, this reaction solution was decanted using a centrifuge and washed until the amount of free fluoride ions was 100 mg/L or less to obtain a niobium-containing precipitate from which the fluoride ions were removed. At this time, ammonia water was used as the washing solution. In addition, a slurry was obtained by diluting the niobium-containing precipitate from which the fluoride ions had been removed with pure water . A portion of this slurry was dried at 110°C for 24 hours and then calcined at 1,000° C for 4 hours to produce Nb₂O₅ , and the amount of Nb₂O₅ contained in the slurry was calculated from the weight. Then, a translucent slurry mixture was obtained by mixing a niobium-containing precipitate slurry diluted with pure water, 5 mass% lithium hydroxide, and pure water. By stirring this mixture and maintaining the liquid temperature at 50°C to 100°C, for example 70°C, for 1 hour, an aqueous solution for neutralizing a niobium compound according to Example 1 was obtained. The niobium content in the aqueous solution for neutralizing a niobium compound according to Example 1 was 2.86 mass%, and the lithium content was 0.23 mass%. (Example 2) In Example 2, 0.29 g of pyrophosphate and 26.85 g of pure water were placed in a polypropylene container, and 2.85 g of a 5 mass% aqueous solution of lithium hydroxide monohydrate was added to the obtained aqueous solution of phosphorus compounds to obtain a mixed solution of phosphorus compounds. Then, 3.02 g of the aqueous solution for neutralizing the niobium compound used in Example 1 was added to the phosphorus compound mixed solution and stirred for 30 minutes to mix, thereby obtaining a niobic acid compound dispersion according to Example 2. In addition, the pyrophosphate and 5 mass% lithium hydroxide monohydrate aqueous solution used in Example 2 are the same as those in Example 1. (Example 3) In Example 3, 0.29 g of pyrophosphate and 25.51 g of pure water were placed