Preparation method of stable water-soluble niobium and tantalum precursor and application thereof

A water-soluble, precursor technology, applied in chemical instruments and methods, niobium compounds, tantalum compounds, etc., can solve problems such as deterioration of photoelectric properties, short service life, and restrictions on the commercial application of precursor systems

Inactive Publication Date: 2005-11-23
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the main disadvantage of the alkoxide-based process is that tantalum ethoxide and niobium ethoxide are expensive and extremely sensitive to moisture. During the preparation process, a strictly dry environment is required, usually in a glove box (Glove box), some chemical reactions Need to be done on a Schlenk vacuum line
The storage of the prepared precursor solution also needs to be waterproof and the service life is short
Although some improvement measures have been adopted, such as the use of ligands such as ethylene glycol methyl ether to replace alkoxy groups, which has partially improved the stability of the precursor, but this problem cannot be fundamentally solved, and it also greatly limits the use of similar precursor systems. commercial application of
Tantalum pentachloride and niobium pentachloride have also been used as precursors of tantalum or niobium, although relative to alkoxides, its price is cheaper and its stability has improved, however, the inevitable small amount of residual chlorine in the final material may can degrade the optoelectronic properties of the material

Method used

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  • Preparation method of stable water-soluble niobium and tantalum precursor and application thereof
  • Preparation method of stable water-soluble niobium and tantalum precursor and application thereof
  • Preparation method of stable water-soluble niobium and tantalum precursor and application thereof

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Embodiment Construction

[0014] 1, the embodiment of the precursor synthesis method of water-soluble niobium:

[0015] Synthetic raw materials: niobium pentoxide (analytical pure, 99.5%), potassium hydroxide or sodium hydroxide (analytical pure), nitric acid (analytical pure), citric acid (analytical pure).

[0016] The synthesis route of water-soluble niobium precursor: mix and grind niobium pentoxide and potassium hydroxide or sodium hydroxide in a molar ratio of 1: (2~20), put them into a corundum crucible, and burn them at 400-550°C for reaction 2 -4 hours, such as burning at 450°C for 2.5-3 hours to obtain a melt of potassium niobate. Dissolve the melt in deionized water, add an appropriate amount of acetic acid to the filtered clear liquid, and a white niobic acid precipitate (Nb 2 o 5 ·nH 2 0), then adjust the pH value to make the solution acidic (PH<4), and the niobium in the solution is completely precipitated in the form of niobic acid. After filtering, the white precipitate was washed r...

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Abstract

The invention provides a preparation method of stable water-soluble niobium and tantalum precursor, which comprises using pentoxide of tantalum or niobium as raw material, mixing columbium pentachloride or ttantalum pentachloride with potassium hydroxide or sodium hydroxide, grinding homogeneously, carrying out incandesce reacting 2-4 hours at 400-550 deg. C, obtaining fusing agent of potassium (sodium) niobate or potassium (sodium) tantalite, dissolving the fluxing agent into deionized water, filtering the solution till the solution shows strong acidity (pH<2), so that the niobium or tantalum in the solution can be fully precipitated in the form of niobic acid or tantalic acid. Finally charging right amount of citric acid water solution into columbic acid or charging right amount of oxalic acid into tantalic acid deposition, thus obtaining water-soluble niobium precursor or oxalate aqueous solution of tantalum.

Description

technical field [0001] The present invention relates to the preparation method of stable water-soluble niobium and tantalum precursor and its application in the preparation of ferroelectric film and powder. Background technique [0002] Ferroelectric materials (such as Sr x Ba 1-x Nb 2 o 6 (SBN), LiNbO 3 , LiTaO 3 , SrBi 2 Ta 2 o 9 (SBT)SrBi 2 Nb 2 o 9 ) is an important class of functional materials with ferroelectric, piezoelectric, pyroelectric, electro-optic, acousto-optic, and nonlinear optical effects, and has broad application prospects in the fields of microelectronics and optoelectronics. Wet chemical methods include sol-gel method (So1-gel), metal organic decomposition method (Metalorganic decomposition, MOD) and chemical solution deposition method (Chemical solution deposition, CSD), etc., and the films and powders prepared by them have high micro-domain components. Uniformity, accurate stoichiometric ratio, easy doping, easy ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00
Inventor 李爱东吴迪闵乃本
Owner NANJING UNIV
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