CaCu3Ti4O12 micro nano sized fiber and its preparation method

A micro-nano fiber technology, applied in fiber processing, spinning solution preparation, filament/thread forming, etc., can solve problems such as difficulties in electrospinning process, inability to carry out electrospinning, and increase in viscosity of spinning solution. Achieve the effect of easy control, mild conditions and wide application

Inactive Publication Date: 2013-07-24
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned technical solution provides fibers for preparing simple oxides, while CaCu 3 Ti 4 O 12 ceramics are composed of three metal elements in fixed proportions Composition, when titanium alkoxides and calcium and copper corresponding inorganic salts are used as raw materials, due to the crystal water contained in the calcium and copper inorganic salts and their own water absorption, the metal alkoxides will quickly Hydrolysis and polymerization, even part of the gel is produced, so that the viscosity of the spinning solution increases geometrically, far beyond the range that can be used for electrospinning. presents difficulties and even makes electrospinning impossible, therefore, the use of CaCu 3 Ti 4 O 12 nanofibers has not been seen so far , in the prior art, there is no report on the preparation of CaCu 3 Ti 4 O 12 micro-nano fibers by electrospinning

Method used

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  • CaCu3Ti4O12 micro nano sized fiber and its preparation method
  • CaCu3Ti4O12 micro nano sized fiber and its preparation method
  • CaCu3Ti4O12 micro nano sized fiber and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0026] 1. Under stirring conditions, add 10 ml of absolute ethanol, 1.04 g of calcium nitrate tetrahydrate and 2.63 g of copper acetate monohydrate into the reaction vessel, and react at a constant temperature of 30°C for 2 hours to obtain solution A;

[0027] 2. Under stirring conditions, add 1.5 g of polyvinylpyrrolidone, 10 ml of absolute ethanol, 3 ml of acetic acid and 6 ml of butyl titanate into the reaction vessel, and react at a constant temperature of 30 ° C for 1 hour to obtain a solution B;

[0028] 3. Under stirring conditions, all the solution B prepared in step 2 was slowly added dropwise to solution A at a rate of 100 ml per hour to obtain solution C;

[0029] 4. Electrospinning solution C, the voltage used for electrospinning is 16.50 kV, the injection rate is 6.5 ml / hour, the curing distance is 12 cm, the receiving device is aluminum foil, and the electrospinning time is 3 hours. corresponding fibers;

[0030] 5. Dry the fiber obtained by electrosp...

Embodiment 2

[0034] 1. Under stirring conditions, add 15 ml of absolute ethanol, 1.04 g of calcium nitrate tetrahydrate and 2.63 g of copper acetate monohydrate into the reaction vessel, and react at a constant temperature of 45°C for 3 hours to obtain solution A;

[0035] 2. Under stirring conditions, add 2.5 grams of polyvinylpyrrolidone, 15 milliliters of absolute ethanol, 1.5 grams of tetramethylammonium hydroxide and 6 milliliters of butyl titanate into the reaction vessel, and react at a constant temperature of 45°C for 3 Hour, obtain solution B;

[0036] 3. Under stirring conditions, slowly add all the solution B prepared in step 2 to solution A at a rate of 200 ml per hour to obtain solution C;

[0037] 4. Electrospinning solution C, the voltage used for electrospinning is 19.50 kV, the injection rate is 8.5 ml / hour, the curing distance is 15 cm, the receiving device is aluminum foil, and the electrospinning time is 2 hours. corresponding fibers;

[0038] 5. Dry the fib...

Embodiment 3

[0040] 1. Under stirring conditions, add 20 ml of absolute ethanol, 2.08 g of calcium nitrate tetrahydrate and 5.26 g of copper acetate monohydrate into the reaction vessel, and react at a constant temperature of 50° C. for 1 hour to obtain solution A;

[0041] 2. Under stirring conditions, add 3 grams of polyvinylpyrrolidone, 20 milliliters of absolute ethanol, 3 grams of tetramethylammonium hydroxide and 12 milliliters of butyl titanate into the reaction vessel, and react at a constant temperature of 50 ° C for 1 Hour, obtain solution B;

[0042] 3. Under stirring conditions, all the solution B prepared in step 2 was slowly added dropwise to solution A at a rate of 150 ml per hour to obtain solution C;

[0043] 4. Electrospinning solution C, the voltage used for electrospinning is 23.50 kV, the injection rate is 9.5 ml / hour, the curing distance is 15 cm, the receiving device is aluminum foil, and the electrospinning time is 2 hours. corresponding fibers;

[0044] ...

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Abstract

The invention discloses a CaCu3Ti4O12 micro nano sized fiber and its preparation method, which belongs to the inorganic material technical field. The CaCu3Ti4O12 micro nano sized fiber comprises the elements of Ca, Cu, Ti and O with the mol ratio of 13412, and the diameter is 200-300 nanometers. The preparation method comprises the following steps mixing anhydrous ethyl alcohol, calcium nitrate tetrahydrate and copper acetate monohydrate to obtain a solution A; mixing anhydrous ethanol, butyl titanate and a spinning auxiliary agent to obtain a solution B; slowly adding the solution B in the solution A, and using a static spinning technology to prepare the CaCu3Ti4O12 micro nano sized fiber. The method of the invention can effectively control the hydrolysis process of the raw materials by selecting and adjusting the ratio of raw materials and the spinning auxiliary agent, the obtained static spinning solution possesses spinnability, and the method of the invention provides the novel CaCu3Ti4O12 micro nano sized fiber. The preparation method has the advantages of simple process, mild condition, easy control and wide applicability.

Description

technical field [0001] The invention relates to an inorganic fiber material technology, in particular to a micro-nano ceramic fiber and a preparation method thereof. Background technique [0002] Materials with high dielectric constant can be used in the manufacture of small-volume capacitive devices, which provides a great possibility for the miniaturization of electronic devices, so it has a wide range of applications in the fields of micro-resonators, filters, mobile phones, etc., in Playing an increasingly important role in the microelectronics industry. [0003] Subramanian et al. (M.A. Subramanian, Dong Li, et al. J. Solid State Chemistry, 2000, 151: 323-325) discovered CaCu with a perovskite-like structure in 2000 3 Ti 4 o 12 (abbreviated as CCTO) has a very high dielectric constant (generally greater than 10,000) in the temperature range of 100-500K, and in a wide temperature range, there is no structural phase transition and ferroelectric phase transitio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/462C04B35/622D01D5/00D01D1/02
Inventor 秦大可顾嫒娟梁国正
Owner SUZHOU UNIV
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