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A kind of preparation method of cacu3ti4o12 film doped with zirconium

A thin film and mixed liquid technology, applied in liquid chemical plating, ceramics, coatings, etc., can solve problems such as difficult to control film stoichiometric ratio, uncontrollable hydrolysis and condensation reactions, expensive equipment and vacuum conditions, etc. It is not easy to achieve Oxygen loss, low cost, and strong bonding effect

Active Publication Date: 2016-01-20
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

If the physical vapor deposition method is used to prepare doped films, although the proportion of doped substances can be strictly controlled, it is not easy to mass-produce because the experiment requires expensive equipment and vacuum conditions, and the cost of material preparation is too high; if the sol-gel method is used , although the cost is low and large-area preparation can be realized, but due to the uncontrollable hydrolysis and condensation reactions in the precursor solution, the stability of the prepared solution is difficult to control, especially in the preparation of multi-component compounds. Various metal alkoxides There is a difference in the speed of the hydrolysis reaction, and it is difficult to control the stoichiometric ratio of various elements in the film, so it is even more difficult to know the amount actually doped into the film. Once the experiment cannot be quantified, it has no practical application value.

Method used

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  • A kind of preparation method of cacu3ti4o12 film doped with zirconium
  • A kind of preparation method of cacu3ti4o12 film doped with zirconium
  • A kind of preparation method of cacu3ti4o12 film doped with zirconium

Examples

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Embodiment 1

[0025] Embodiment 1: a kind of CaCu doped with zirconium 3 Ti 4 o 12 The preparation method of thin film, comprises the steps:

[0026] Step 1: Prepare a mixed solution containing calcium-copper-titanium. Specifically include the following steps:

[0027] (1) At room temperature, add 2g of inorganic Ca(NO 3 ) 2 salt to obtain a mixed solution A, add 2g of water-soluble polymer polyethyleneimine (PEI) with amino groups and 2g of stabilizing complexing agent ethylenediaminetetraacetic acid (EDTA) to solution A, ultrasonic and stir until The solution was clear and transparent, and mixed solution B was obtained. Use an ultrafiltration device to filter out free ions in solution B, and evaporate and concentrate to obtain calcium-containing mixed solution X with a concentration of 103.03 mmol / L;

[0028] (2) Add 2g Cu(NO 3 ) 2 To obtain mixed solution C, add 2gPEI macromolecule and 2gEDTA to solution C and ultrasonically stir to obtain mixed solution D, filter mixed solution...

Embodiment 2

[0041] The difference between this example and Example 1 is that in step 3, 0.48mL of zirconium-containing mixed solution I is taken, and added to the calcium-copper-titanium mixed solution obtained in step 1, fully mixed, stirred, and ultrasonically obtained to obtain a 10% molar ratio doped Zr 4+ calcium copper titanium zirconium precursor.

[0042] Below to the CaCu that embodiment 2 obtains 3 Ti 4 o 12 Analysis of the structure and properties of the film:

[0043] figure 2 (b) CaCu obtained for Example 2 3 Ti 4 o 12 The X-ray diffraction (XRD) θ-2θ scanning pattern of the film, which is shown on the single crystal substrate LaAlO 3 Successfully prepared CaCu doped with zirconium ions 3 Ti 4 o 12 Thin film, CaCu doped with zirconium ions 3 Ti 4 o 12 The CCTO (004) peak of the film compared with 0% doped CaCu 3 Ti 4 o 12 The film phase shifts to the left, indicating that the doped CaCu 3 Ti 4 o 12 The film unit cell becomes larger.

[0044] Figure 4 (...

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Abstract

The invention discloses a method for preparing a zirconium-doped CaCu3Ti4O12 thin film, which belongs to the technical field of dielectric material synthesis. The method includes the following steps: 1) preparing a calcium-copper-titanium-containing mixed solution according to the molar ratio of calcium, copper and titanium at a ratio of 1:3:4; 2) preparing a zirconium-containing mixed solution, adding Calcium-copper-titanium-zirconium-containing precursor solution was obtained; 3) The substrate was placed in a tube furnace, heated to 900°C and kept for 10 hours, and then cooled down to room temperature naturally with the furnace; and then spin-coated The precursor liquid containing calcium copper titanium zirconium is coated on the substrate, and dried to obtain the thin film sample containing calcium copper titanium zirconium; 4) The thin film sample obtained in step 3) is placed in a tube furnace and heated at 900 ° C in an oxygen atmosphere Under heat treatment for 10 hours, the zirconium-doped CaCu3Ti4O12 thin film was obtained with the furnace cooling down. The method of the invention can accurately control the doping amount of Zr4+ in the thin film, and at the same time, the dielectric loss is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of dielectric material synthesis, in particular to a zirconium-doped CaCu 3 Ti 4 o 12 The method of film preparation. Background technique [0002] The development and research of high dielectric constant materials (ε>1000) has brought rapid development to the application of large-capacity capacitors and the miniaturization and miniaturization of electronic components. So far, some high dielectric constant materials have been applied in practical devices. CaCu was discovered in 2000 3 Ti 4 o 12 (CCTO) under the action of 1kHz AC electric field, the dielectric constant can reach 12,000, and in the temperature range from 100K to 400K, the dielectric constant is basically unchanged, and the low-frequency dielectric constant of its single crystal sample can even reach 10 5 . Once the high dielectric properties of CCTO were discovered, it immediately attracted widespread attention. However, the dielect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C18/12H01B3/12
Inventor 林媛冯大宇高敏张胤
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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