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PST[(pB, sR)tIo3] and its Ba solution, Mg/Mn/K doping material system preparing method

A technology for doping materials and solutions, applied in metal material coating process, liquid chemical plating, coating, etc., which can solve the problems of increased operation steps and operation time, low yield of PST sol, and increased cost of preparation facilities. Achieve the effect of long preservation period, high efficiency and waste reduction

Inactive Publication Date: 2009-01-14
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the sol prepared by M.Jain et al. needs to boil and heat the solution at 110°C to remove crystallization water, which will cause air pollution or increase the cost of preparation facilities; in addition, various acetates must be dissolved separately during the preparation process. , which increases the operation steps and operation time, thereby reducing the yield
The PST sol yield prepared by DongHeon Kang et al. is lower, because the preparation of each sol requires low temperature heating for 24 hours

Method used

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  • PST[(pB, sR)tIo3] and its Ba solution, Mg/Mn/K doping material system preparing method
  • PST[(pB, sR)tIo3] and its Ba solution, Mg/Mn/K doping material system preparing method
  • PST[(pB, sR)tIo3] and its Ba solution, Mg/Mn/K doping material system preparing method

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Effect test

Embodiment 1

[0014] Embodiment 1: the preparation of PST powder

[0015]Dissolve Pb and Sr acetate in glacial acetic acid at 40-120°C, mix ethylene glycol methyl ether and tetrabutyl titanate with a content of 0-40V%, and mix the two solutions at 40-120°C Mix and stir, then add ethylene glycol, adjust the amount of glacial acetic acid so that the final concentration of PST is 0.1-0.5mol / L, filter after 0.1-5 hours of heat preservation, and obtain a clear and transparent sol. Glycol: ethylene glycol methyl ether: glacial acetic acid dissolves acetate and tetrabutyl titanate at a ratio of 1:0.5 to 5:7 to 14.

[0016] Heat the obtained PST sol in a horse boiling furnace at a rate of 5-20°C / min to a temperature between 200-600°C for 0.1-3 hours, and then heat it to a temperature of 600-600°C at a rate of 5-20°C / min. Insulate at 900°C for 0.1-3 hours, and then cool down to room temperature with the furnace, and the perovskite PST powder with perfect crystallization and no impurity phase can be...

Embodiment 2

[0018] Pb 0.25 Ba 0.15 Sr 0.8 TiO 3 The preparation process of the sol is as follows: the acetates of Pb, Sr and Ba are dissolved in glacial acetic acid, and the dissolution temperature is 40-120°C. Mix ethylene glycol methyl ether and tetrabutyl titanate with a content of 0-40V% evenly. Mix and stir the above two solutions at a temperature of 40-120°C, then add ethylene glycol, and adjust the amount of glacial acetic acid so that Pb 0.25 Ba 0.15 Sr 0.6 TiO 3 The final content is 0.5mol / L. Filtrate after heat preservation for 0.1-5 hours to obtain a clear and transparent solution.

[0019] Pb 0.25 Ba 0.15 Sr 0.6 TiO 3 Thin films were prepared as follows: on Pt / TiO 2 / SiO 2 On the Si substrate, make a thin film at a speed of 250-6000r / min, heat the film at a speed of 1-100°C / min to a certain temperature of 200-600°C for 0.1-3 hours, and then heat it at 5-100°C / min Raise the temperature at a rate of 600-900°C for 0.1-3 hours, and then cool down to room temperature...

Embodiment 3

[0025] K-doped PST is PKST[(Pb, K, Sr)TiO 3 ]’s sol synthesis, thin film preparation, top electrode preparation and final performance test are basically similar to those of PBST, the only difference is that the acetate of Ba is changed to the acetate of K and the content of ethylene glycol methyl ether is changed. Minor changes. Here, the synthesis of PKST and the preparation of thin films will not be repeated here.

[0026] Scanning electron micrographs show that 2.5% K-doped Pb 0.3 Sr 0.7 TiO 3 Afterwards, the grain size increases significantly. This change should affect the Pb 0.3 Sr 0.7 TiO 3 have a great influence on the dielectric properties.

[0027] Figure 4 for (Pb 0.3 Sr 0.7 ) 0.975 K 0.025 TiO 3 and Pb 0.3 Sr 0.7 TiO 3 The tuning spectrum of the dielectric parameters as a function of bias voltage. Depend on Figure 4 It can be seen that after 2.5% K doping Pb 0.3 Sr 0.7 TiO 3 After that, the dielectric parameters have increased several times, ...

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Abstract

The invention discloses a method to make PST [(Pb, Sr) TiO3] and Ba solid solvent Mg / Mn / K doping material system by sol gel technology. It dissolves Pb, Sr or Pb, SR, Ba or Pb, Sr and acetate of Mg / Mn / K into glacial acetic acid, equally mixes 0-40V% ethylene glycol monomethyl ether with butyl titanate, whisking the mixture under 40-120 degree centigrade and adding glycol, adjusts the content of glacial acetic acid, heating under certain temperature, filtering, dissolving glue and annealing and crystallizing. The PST and Ba solid liquid, Mg / Mn / K doping material system film or powder would be gained. The invention has simple steps, and low compounding temperature. It establishes a foundation for microwave tune component.

Description

technical field [0001] The present invention relates to a kind of PST[(Pb, Sr)TiO prepared by sol-gel process 3 ] and its Ba solid solution, Mg / Mn / K doped material method, the method prepares PST and its Ba solid solution, Mg / Mn / K doped material system powder or film with an improved sol-gel process, especially The invention relates to a novel dielectric film suitable for preparing a microwave phase shifter and an uncooled infrared detection focusing coplanar array, and belongs to the field of ferroelectric dielectric materials and also belongs to the field of preparation of electronic components. Background technique [0002] PST is PbTiO 3 and SrTiO 3 Infinite solid solution of PST is possessed of PbTiO 3 The high dielectric parameter of SrTiO 3 It has high structural stability, and the Curie temperature and dielectric constant can be adjusted almost linearly with Pb / Sr. Its processing temperature is much lower than that of BST, and it also has relatively low dielectri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C18/02B22F9/30
Inventor 赵兴中孙小华刘威韩宏伟
Owner WUHAN UNIV
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