Preparation method of Magneli phase low valence titanium oxide

A technology of oxide and low-valent titanium, which is applied in the field of preparation of Magnéli phase low-valent titanium oxide materials, can solve the problems of high cost of Magnéli phase materials, harsh reaction conditions, and high calcination temperature, and achieve the effect of saving production costs

Active Publication Date: 2017-06-13
马根英
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction conditions of the above two methods are very harsh, the calcination temperature is high, the calcination time is long, and the inert gas needs to be continuou

Method used

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  • Preparation method of Magneli phase low valence titanium oxide
  • Preparation method of Magneli phase low valence titanium oxide
  • Preparation method of Magneli phase low valence titanium oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The mass percentage of the main raw materials aluminum powder and titanium dioxide used in the implementation of Example 1 is: 0.56:1.

[0042] S101: Weigh 50 g of titanium dioxide and 28 g of aluminum powder, add 25 mL of absolute ethanol, mill the weighed titanium dioxide, aluminum powder, and absolute ethanol in a planetary ball mill for 1 hour, and mix well.

[0043] S102: Put the raw material mixed in S101 into the crucible for compaction, and cover the surface of the raw material with a layer of molten B 2 o 3 , a thickness of 3mm, to isolate the air.

[0044] S103: Prepare three identical samples according to the steps of S101 and S102, which are samples a, b, and c respectively.

[0045]S104: Put the samples prepared in S103 into a box-type resistance furnace for roasting, the roasting temperature is 950°C, and the roasting time is 20 min, 25 min, and 30 min respectively, and naturally cool in the air atmosphere after the reaction is completed.

[0046] The m...

Embodiment 2

[0054] The mass percentage of the main raw materials aluminum powder and titanium dioxide used in the implementation of Example 2 is: 0.56:1.

[0055] S101: Weigh 50 g of titanium dioxide and 28 g of aluminum powder, add 30 mL of absolute ethanol, mill the weighed titanium dioxide, aluminum powder, and absolute ethanol in a planetary ball mill for 1 hour, and mix well.

[0056] S102: Put the raw material mixed in S101 into the crucible for compaction, and cover the surface of the raw material with a layer of molten B 2 o 3 , a thickness of 4mm, to isolate the air.

[0057] S103: Put the crucible prepared in S102 into a box-type resistance furnace for calcination, the calcination temperature is 850° C., and the calcination time is 30 minutes. After the reaction is completed, it is naturally cooled in an air atmosphere.

[0058] S104: leaching the prepared material in hydrochloric acid with a concentration of 15%, the leaching time is 10 min, and the stirring speed is 60 rpm. ...

Embodiment 3

[0061] The mass percentage of the main raw materials aluminum powder and titanium dioxide used in the implementation of Example 3 is: 0.68:1.

[0062] S101: Weigh 50 g of titanium dioxide and 34 g of aluminum powder, add 30 mL of absolute ethanol, mill the weighed titanium dioxide, aluminum powder, and absolute ethanol in a planetary ball mill for 1 hour, and mix well.

[0063] S102: Put the raw material mixed in S101 into the crucible for compaction, and cover the surface of the raw material with a layer of molten B 2 o 3 , a thickness of 5mm, to isolate the air.

[0064] S103: Put the crucible prepared in S102 into a box-type resistance furnace for calcination, the calcination temperature is 1000° C., and the calcination time is 10 minutes. After the reaction is completed, cool naturally in the air atmosphere.

[0065] S104: leaching the prepared material in dilute sulfuric acid with a concentration of 20%, for 10 minutes, and at a stirring rate of 60 rpm.

[0066] Implem...

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Abstract

The invention relates to the technical field of inorganic material preparation process, in particular to a preparation method of Magneli phase low valence titanium oxide. The method comprises the steps of uniformly mixing titanium pigment, aluminum powder and absolute ethanol in the mass and volume ratio of 0.4-0.8g: 1g: 0.5-0.8mL, adding the uniformly mixed material into a crucible to compaction, melting boron oxide with low melting point, using the boron oxide to cover the material surface, putting the crucible on an electric heating furnace for roasting to obtain the low valence titanium oxide. Because the Magneli phase low valence titanium oxide is stable in chemical property, the finally obtained material is leached in acid to obtain the pure Magneli phase (TinO2n-1) low valence titanium oxide. According to the Magneli phase low valence titanium oxide, the preparation in relatively low temperature, normal pressure and relatively short period of time is achieved, the cost is greatly reduced, and the method is beneficial to achieve the scale production and preparation.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic materials, in particular to a Magnéli phase (Ti n o 2n-1 ) A method for preparing a low-valent titanium oxide material. Background technique [0002] Ti n o 2n-1 (4<n<10) is a series of substoichiometric oxides of titanium, which have many excellent properties such as good electrical conductivity, strong visible light response ability, excellent electrochemical performance, environmental protection and non-toxicity. Among them, Ti 4 o 7 The conductivity of single crystal reaches 1500S cm -1 , comparable to graphite. Ti n o 2n－1 A lot of progress has been made in the phase structure, electromagnetism and electrochemistry of the phase structure. Due to its excellent properties, Ti n o 2n-1 Applications in inert electrodes, catalyst supports, lithium batteries, thermoelectric and photoelectric materials, and photocatalytic degradation have attracted the attention of...

Claims

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Application Information

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IPC IPC(8): C01G23/04
CPCC01G23/043C01P2002/72
Inventor 李军吴恩辉侯静杨绍利赖奇黄平徐纵刘黔蜀
Owner 马根英
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