Iodometric method for determining oxygen vacancy concentration in barium ferrite-based lead-free piezoelectric ceramics

A lead-free piezoelectric and bismuth ferrite technology is used in chemical analysis by titration, which can solve the problems of inaccurate, different, and measurement errors in experimental results, and achieve simple operation steps, easy operation, and simple experimental instruments. Effect

Active Publication Date: 2019-01-01
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the color resolution ability of different people is different, and bismuth ferrite-based lead-free piezoelectric ceramics is an insulating material, which contains less oxygen vacancies. When judging the color with the naked eye to determine the titration

Method used

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  • Iodometric method for determining oxygen vacancy concentration in barium ferrite-based lead-free piezoelectric ceramics
  • Iodometric method for determining oxygen vacancy concentration in barium ferrite-based lead-free piezoelectric ceramics
  • Iodometric method for determining oxygen vacancy concentration in barium ferrite-based lead-free piezoelectric ceramics

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Experimental program
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preparation example Construction

[0083] 1. Preparation of standard samples

[0084] Weigh 0.0564g-3.1447g of bismuth oxide and 0.0194g-1.0778g of iron oxide, add 5mL-280mL of concentrated hydrochloric acid, stir with a magnetic stirrer until completely dissolved, and obtain the required solution.

[0085] 2. Determine the color spectrum of the standard sample

[0086] Add 0.1000~5.5557gKI to the solution in step 1, then titrate the sodium thiosulfate standard solution, add starch indicator when the color becomes light, and it is dark blue at this time, continue to titrate the sodium thiosulfate solution, when the blue color disappears, The titration is over. Write down the color change at each stage, and measure the color spectrum at each stage with a spectrophotometer.

[0087] Such as figure 2 As shown, according to a kind of iodine method for measuring the oxygen vacancy concentration in the bismuth ferrite-based lead-free piezoelectric ceramics according to the present invention, it specifically inclu...

Embodiment 1

[0117] In this embodiment, a set of (1-z) BiFeO 3 -zBaTiO 3 (z=0.20, 0.25, 0.30, 0.35, 0.4) sample as an example, the specific determination method steps are as follows:

[0118] 1. Sample weighing

[0119] Take 0.7BiFeO 3 -0.3BaTiO 3 (z=0.30) ceramic samples were ground into powder with an alumina mortar, and 0.1000 g of powder samples were accurately weighed with an electronic balance.

[0120] 2. Sample dissolution

[0121] Put the weighed powder sample in a 100mL three-neck round-bottomed flask, add 5mL of concentrated hydrochloric acid, and stir with a magnetic stirrer until the bottom of the solution is all white precipitate, which is barium titanate, which is insoluble in concentrated hydrochloric acid. At this time, the solution is Brown yellow, transfer the sodium thiosulfate standard solution to the burette with a pipette, and read the scale number V 1 .

[0122] 3. Sample titration

[0123] Add 0.1000g of potassium iodide to the solution, immediately cover t...

Embodiment 2

[0148] In this embodiment, a set of 0.7Bi(Fe 1-y m y )O 3 -0.3BaTiO 3 (M=Sc; y=0.00, 0.02, 0.04, 0.06, 0.08) sample as an example, the specific determination method steps are as follows:

[0149] 1. Sample weighing

[0150] Take 0.7BiFeO 3 -0.3BaTiO 3 (y=0.00) ceramic samples were ground into powder with an alumina mortar, and 0.6032 g of powder samples were accurately weighed with an electronic balance.

[0151] 2. Sample dissolution

[0152] Put the weighed powder sample in a 100mL three-necked flask, add 30mL of concentrated hydrochloric acid, and stir with a magnetic stirrer until the bottom of the solution is all white precipitate, the white precipitate is barium titanate, which is insoluble in concentrated hydrochloric acid, and the solution is brown at this time , move the sodium thiosulfate standard solution to the burette with a pipette, and read the scale number V 1 .

[0153] 3. Sample titration

[0154] Add 0.6000g of potassium iodide to the solution, imm...

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Abstract

The invention discloses an iodometric method for determining oxygen vacancy concentration in barium ferrite-based lead-free piezoelectric ceramics, belonging to the technical field of ceramic composition analysis. The method comprises the following steps: taking a ceramic sample and grinding into a powder, weighing in a round-bottom flask; adding concentrated hydrochloric acid and stirring until the powder is completely dissolved, and marking the obtained solution in brown yellow color; adding a sodium thiosulfate standard solution into a burette, recording the number of the scale; adding potassium iodide into the brown yellow solution and covering with a plug; vacuuming and then introducing nitrogen gas, stirring evenly, and marking the obtained solution in reddish brown color; titratingto be light brown yellow with the sodium thiosulfate standard solution, adding a starch solution, and marking the obtained solution with dark blue; using the sodium thiosulfate standard solution to titrate until the blue color disappears; recording the numbers of the scales after the twice addition of the sodium thiosulfate standard solution, and calculating the total consumption amount of the sodium thiosulfate standard solution; calculating the valence state of Fe ions in the ceramic sample, and then utilizing charge balance to obtain the oxygen vacancy concentration. The iodometric method provided by the invention is simple and convenient in experimental instruments, simple to operate and accurate and reliable in detection results, and can realize the quantitative analysis of the oxygenvacancy concentration.

Description

technical field [0001] The invention belongs to the technical field of ceramic component analysis, and in particular relates to an iodometric method for measuring the concentration of oxygen vacancies in bismuth ferrite-based lead-free piezoelectric ceramics. Background technique [0002] Piezoelectric ceramics are a class of functional materials with piezoelectric effect, which can realize mutual conversion between mechanical energy and electrical energy, so they are widely used in aerospace, military and medical fields. Bismuth ferrite is a high-temperature ferroelectric, which has both ferroelectricity and ferromagnetism above room temperature. Its Curie temperature is 830°C, Neel temperature is 370°C, and its theoretical spontaneous polarization is about 100μC / cm 2 , is the research focus of lead-free piezoelectric ceramics in recent years. However, the synthesis temperature range of bismuth ferrite is narrow, and bismuth oxide is easily volatilized during sintering to ...

Claims

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Application Information

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IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 张波萍唐宇成荀勃伟
Owner UNIV OF SCI & TECH BEIJING
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